CN1676679A - Up-conversion laser crystal Er3+,Yb3+,Na+:CaF2 - Google Patents
Up-conversion laser crystal Er3+,Yb3+,Na+:CaF2 Download PDFInfo
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- CN1676679A CN1676679A CN 200510023473 CN200510023473A CN1676679A CN 1676679 A CN1676679 A CN 1676679A CN 200510023473 CN200510023473 CN 200510023473 CN 200510023473 A CN200510023473 A CN 200510023473A CN 1676679 A CN1676679 A CN 1676679A
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- infrared
- conversion laser
- laser crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 72
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 30
- 229910001634 calcium fluoride Inorganic materials 0.000 title abstract 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 229910004261 CaF 2 Inorganic materials 0.000 claims description 28
- 230000012010 growth Effects 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 9
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 abstract description 8
- 238000005086 pumping Methods 0.000 abstract description 8
- 229910016495 ErF3 Inorganic materials 0.000 abstract 1
- 229910009520 YbF3 Inorganic materials 0.000 abstract 1
- FPHIOHCCQGUGKU-UHFFFAOYSA-L difluorolead Chemical compound F[Pb]F FPHIOHCCQGUGKU-UHFFFAOYSA-L 0.000 abstract 1
- 239000000155 melt Substances 0.000 abstract 1
- QGJSAGBHFTXOTM-UHFFFAOYSA-K trifluoroerbium Chemical compound F[Er](F)F QGJSAGBHFTXOTM-UHFFFAOYSA-K 0.000 abstract 1
- 238000000295 emission spectrum Methods 0.000 description 8
- 241000209456 Plumbago Species 0.000 description 7
- 229910052691 Erbium Inorganic materials 0.000 description 6
- 229910052769 Ytterbium Inorganic materials 0.000 description 6
- 230000010354 integration Effects 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 229940123973 Oxygen scavenger Drugs 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- -1 rare earth ion Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
Er3+,Yb3+And Na+Co-doped CaF2The infrared up-conversion laser crystal is characterized by comprising the following components: raw materials: the molar ratio is as follows: ErF3:0.005~0.1;YbF3:0.02~0.2;NaF:0.01~0.2;CaF2:1.0;PbF2: 0 to 0.01. Growing by a melt method. The upconversion laser crystal of the present invention can be usedThe commercialized InGaAs laser diode is used as a very effective pumping light source, and the integral intensity of up-conversion luminescence is improved by ten times under the same pumping condition.
Description
Technical field
The present invention relates to up-conversion laser crystal, particularly a kind of Er
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal, it is laser diode-pumped that it is suitable for InGaAs.
Background technology
In recent years, rare earth ion doped various solid material up-conversion luminescences promptly absorbed infrared pump light and the research of visible emitting is very extensive.Based on the high-performance of infra-red laser diode LD pumping source, such up-conversion lasing material shows at colour, optical storage, and medical diagnosis, transmitter, there is the potential application prospect in a plurality of fields such as seabed optical communication.Multiple rare earth ion such as Er
3+, Tm
3+, Ho
3+Deng the up-conversion luminescence performance furtherd investigate Er wherein
3+Last efficiency of conversion the highest, relevant research is also at most (with reference to Optics Letters, 22:1412,1997; Applied PhysicsLetters, 80:4510,2002; Journal of Applied Physics, 95:3020,2004).The characteristic of substrate material also is an important factor that influences up-conversion luminescence efficient.
Compare with oxide crystal, fluorochemical has much lower phonon energy, can reduce the radiationless transition probability that causes because of the multi-phonon relaxation widely.Crystal of fluoride such as LiYF with low-symmetry
4, BaY
2F
8Deng comparing CaF
2Has lower phonon energy (328cm
-1), higher thermal conductivity (10Wm
-1K
-1) and better mechanical property, and obtain large-sized single crystal quite easily.Therefore, also had in early days about Er
3+: CaF
2The research of crystalline up-conversion luminescence is (with reference to Journal of Applied Physics, 60:4077,1986; Solid State Communications, 94:379,1995).But, because Er
3+Lack pump absorption band efficiently at infrared band, must ion co-doped with sensitized.To Er
3+The sensitized ions that energy transfer efficiency is the highest is the Yb of available high-octane InGaAs laser diode (LD) pumping
3+Ion, but at CaF
2The Yb ion is very easy to form divalent state (with reference to Physical Review, 184:348,1969) in the lattice, thereby reduces energy transfer efficiency.
In sum, if can be at good host crystal CaF
2The middle Yb that realizes
3+→ Er
3+High efficiency pump energy shift, just can obtain high efficiency up-conversion luminescence.
Summary of the invention
Main purpose of the present invention is to seek a kind of laser diode-pumped high efficiency infrared up-conversion luminous material that is suitable for, and a kind of Er is provided
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal, wherein Yb
3+As sensitized ions, play and shift pump energy to Er
3+Effect; Na
+As the charge compensation ionic simultaneously, play prevention Yb
3+Cluster structure and Yb
2+The effect that forms, thus Yb improved widely
3+→ Er
3+The pump energy transfer efficiency.
Specific embodiment of the present invention is as follows:
A kind of Er
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal is characterised in that it is composed as follows:
Material molar ratio
ErF
3 0.005~0.1
YbF
3 0.02~0.2
NaF 0.01~0.2
CaF
2 1.0
PbF
2 0~0.01
The preferred span of described NaF is: 0.04~0.15.
The optimum valuing range of described NaF is: 0.06~0.1.
Described PbF
2Span be 0.002~0.004.
Described Er
3+, Yb
3+And Na
+The CaF that mixes altogether
2The growth method of infrared up-conversion laser crystal is characterized in that adopting melt method for growing, and its concrete steps are as follows:
Selected formula rate takes by weighing all raw materials, and thorough mixing is the back briquetting evenly, in the crucible of packing into then, adopts the above-mentioned single crystal of melt method for growing.
Described melting method is a crystal pulling method, or falling crucible method, or temperature gradient method.
Described crystal pulling method, crucible material are iridium, and it is the CaF of [111] that seed crystal adopts through X-ray diffractometer accurate pointing normal line of butt end direction
2Single crystal rod, crystal growth is at high-purity inert atmosphere or fluorine-containing atmosphere (CF
4Or HF) carries out in.
Described falling crucible method or temperature gradient method, crucible material adopts high purity graphite, and crucible bottom can not put seed crystal, or puts into the CaF described in the above-mentioned crystal pulling method
2Single crystal rod, crystal growth be in high vacuum, high-purity Ar atmosphere or fluorine-containing atmosphere (CF
4Or HF) carries out in.
Characteristics of the present invention are that this up-conversion laser crystal can adopt business-like InGaAs laser diode as highly effective pump light source, Na
+The integrated intensity that makes its up-conversion luminescence under identical pumping condition that mixes improve tens of times.This crystal can be used for developing efficiently changes visible laser on the LD pumped all-solid-state.
Description of drawings
Figure 1 shows that crystal Er (1.7mol%), Yb (4.3mol%), Na (8.9mol%): CaF
2Room temperature absorption spectrum in 400~1700nm wavelength region.
Curve A is depicted as Er (1.7mol%) among Fig. 2, Yb (4.3mol%), Na (8.9mol%): CaF
2Crystal at wavelength be record under the laser diode-pumped effect of InGaAs of 980nm on switching emission spectrum.Curve B is the Er that records under the same terms
3+(1.7mol%), Yb
3+(4.3mol%): CaF
2Switching emission spectrum on the crystalline, its intensity have been exaggerated 10 times.
Embodiment
The invention will be further described below by embodiment
Embodiment 1: Czochralski grown [Er, Yb, Na:CaF
2] crystal
Press ErF
3, YbF
3, NaF, CaF
2Mol ratio be 0.005: 0.002: 0.01: 0.983 takes by weighing raw material, mixes back briquetting on hydropress, is put in the iridium crucible, adopts Czochralski grown crystal, and it is the CaF of [111] that seed crystal adopts through X-ray diffractometer accurate pointing normal line of butt end direction
2Single crystal rod, crystal growth is in high-purity N
2Carry out in the atmosphere.
Embodiment 2: warm terraced method growth [Er, Yb, Na:CaF
2] crystal
Press ErF
3, YbF
3, NaF, CaF
2Mol ratio be 0.009: 0.045: 0.045: 0.9 prepares burden, and adds the PbF that content is 0.002mol then
2As Oxygen Scavenger, mix back briquetting on hydropress, be put in the plumbago crucible, crucible bottom does not have seed crystal.Adopt temperature gradient method, growing crystal in high vacuum atmosphere.
Embodiment 3: warm terraced method growth [Er, Yb, Na:CaF
2] crystal
Press ErF
3, YbF
3, NaF, CaF
2Mol ratio be 0.017: 0.043: 0.089: 0.85 takes by weighing raw material, adds the PbF that content is 0.006mol then
2As Oxygen Scavenger.Raw material mixes back briquetting on hydropress, is put in the plumbago crucible, and crucible bottom is placed with through the CaF of X-ray diffractometer accurate pointing normal line of butt end direction for [111]
2Single crystal rod is as seed crystal.The plumbago crucible that installs raw material is put into temperature gradient furnace, growing crystal in high-purity Ar atmosphere.The crystal-cut of being grown is in blocks, test the room temperature absorption spectrum as shown in Figure 1 behind the optical polish on Jasco V-570 UV/VIS/NIR spectrophotometer, wherein the strong absorption band of 900~1000nm wave band helps adopting the InGaAs laser diode to carry out pumping.Switching emission spectrum on test room temperature on the Triax550 fluorescence spectrophotometer, it is the InGaAs laser diode of 980nm that pumping source adopts wavelength, the fluorometric investigation scope is visible-range 500~700nm.The curve A of Fig. 2 is depicted as the Er (1.7mol%) that records, Yb (4.3mol%), Na (8.9mol%): CaF
2Switching emission spectrum on the crystalline.In order to compare, the curve B of Fig. 2 has shown the Er that records under the same conditions
3+(1.7mol%), Yb
3+(4.3mol%): CaF
2Switching emission spectrum on the crystalline, its intensity have been exaggerated 10 times.Curve A equals 31.4 with the ratio of the green intensity integration of curve B; The ratio of both red light intensity integrations equals 39.3; The ratio of both red-green glow intensity integration sums equals 36.2.
Embodiment 4: Bridgman-Stockbarge method for growing [Er, Yb, Na:CaF
2] crystal
Press ErE
3, YbF
3, NaF, CaF
2Mol ratio be 0.037: 0.074: 0.148: 0.74 takes by weighing raw material, adds the PbF that content equals 0.01mol then
2As Oxygen Scavenger.Raw material mixes back briquetting on hydropress, is put in the plumbago crucible, and crucible bottom is placed with through the CaF of X-ray diffractometer accurate pointing normal line of butt end direction for [111]
2Single crystal rod is as seed crystal.The plumbago crucible that installs raw material is put into crucible decline stove, at CF
4Growing crystal in the reaction atmosphere.
Embodiment 5: Czochralski grown [Er, Yb, Na:CaF
2] crystal
Press ErF
3, YbF
3, NaF, CaF
2Mol ratio be 0.061: 0.115: 0.061: 0.76 takes by weighing raw material, adds the PbF that content is 0.008mol then
2As Oxygen Scavenger.Raw material mixes back briquetting on hydropress, is put in the iridium crucible, adopts Czochralski grown crystal, and it is the CaF of [111] that seed crystal adopts through X-ray diffractometer accurate pointing normal line of butt end direction
2Single crystal rod, crystal growth is carried out in high-purity Ar atmosphere.
Embodiment 6: Bridgman-Stockbarge method for growing [Er, Yb, Na:CaF
2] crystal
Press ErF
3, YbF
3, NaF, CaF
2Mol ratio be 0.069: 0.138: 0.103: 0.69 takes by weighing raw material, adds the PbF that content is 0.003mol then
2As Oxygen Scavenger.Mix back briquetting on hydropress, be put in the plumbago crucible, crucible bottom is placed with through the CaF of X-ray diffractometer accurate pointing normal line of butt end direction for [111]
2Single crystal rod is as seed crystal.The plumbago crucible that installs raw material is put into crucible decline stove, growing crystal in high-purity Ar atmosphere.
The foregoing description after tested, typical characteristics is as shown in Figure 2.With the Yb of embodiment 3 growths, Na:CaF
2The single crystal dicing is being tested switching emission spectrum on the room temperature behind the optical polish on the Triax550 fluorescence spectrophotometer, it is the InGaAs laser diode of 980nm that pumping source adopts wavelength, and the fluorometric investigation scope is visible-range 500~700nm.The curve A of Fig. 2 is depicted as the Er (1.7mol%) that records, Yb (4.3mol%), Na (8.9mol%): CaF
2Switching emission spectrum on the crystalline.In order to compare, the curve B of Fig. 2 has shown the Er that records under the same conditions
3+(1.7mol%), Yb
3+(4.3mol%): CaF
2Switching emission spectrum on the crystalline, its intensity have been exaggerated 10 times.As seen from the figure, mainly to have two emission band: 510~570nm be green glow in up-conversion luminescence; 630~690nm is a ruddiness.Curve A equals 31.4 with the ratio of the green intensity integration of curve B; The ratio of both red light intensity integrations equals 39.3; The ratio of both red-green glow intensity integration sums equals 36.2.This shows, at Er
3+, Yb
3+: CaF
2Mix a certain amount of Na in the crystal
+Can improve Er widely
3+Up-conversion luminescence intensity.
Claims (8)
1, a kind of Er
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal is characterised in that it is composed as follows:
Material molar ratio
ErF
3 0.005~0.1
YbF
3 0.02~0.2
NaF 0.01~0.2
CaF
2 1.0
PbF
2 0~0.01
2, Er according to claim 1
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal is characterized in that the span of described NaF is: 0.04~0.15.
3, Er according to claim 2
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal, the span that it is characterized in that described NaF is 0.06~0.1.
4, Er according to claim 2
3+, Yb
3+And Na
+The CaF that mixes altogether
2Infrared up-conversion laser crystal is characterized in that described PbF
2Span be 0.002~0.004.
5, the described Er of claim 1
3+, Yb
3+And Na
+The CaF that mixes altogether
2The growth method of infrared up-conversion laser crystal is characterized in that adopting melt method for growing, and its concrete steps are as follows:
Selected formula rate takes by weighing all raw materials, and thorough mixing is the back briquetting evenly, in the crucible of packing into then, adopts the above-mentioned single crystal of melt method for growing.
6, Er according to claim 5
3+, Yb
3+And Na
+The CaF that mixes altogether
2The growth method of infrared up-conversion laser crystal is characterized in that described melting method is a crystal pulling method, or falling crucible method, or temperature gradient method.
7, Er according to claim 6
3+, Yb
3+And Na
+The CaF that mixes altogether
2The growth method of infrared up-conversion laser crystal is characterized in that described crystal pulling method, and crucible material is an iridium, and it is the CaF of [111] that seed crystal adopts through X-ray diffractometer accurate pointing normal line of butt end direction
2Single crystal rod, crystal growth is carried out in high-purity inert atmosphere or fluorine-containing atmosphere.
8, Er according to claim 6
3+, Yb
3+And Na
+The CaF that mixes altogether
2The growth method of infrared up-conversion laser crystal is characterized in that described falling crucible method or temperature gradient method, and crucible material adopts high purity graphite, and crucible bottom can not put seed crystal, or puts into the CaF described in the above-mentioned crystal pulling method
2Single crystal rod, crystal growth are carried out in high-purity Ar atmosphere or the fluorine-containing atmosphere in high vacuum.
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CNB2005100234734A CN1298895C (en) | 2005-01-20 | 2005-01-20 | Up-conversion laser crystal Er3+,Yb3+,Na+:CaF2 |
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Publication Number | Publication Date |
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CN1676679A true CN1676679A (en) | 2005-10-05 |
CN1298895C CN1298895C (en) | 2007-02-07 |
Family
ID=35049418
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008169065A (en) * | 2007-01-10 | 2008-07-24 | Tohoku Univ | Fluoride bulk single crystal material for up-conversion |
CN102534776A (en) * | 2012-03-30 | 2012-07-04 | 中国科学院上海硅酸盐研究所 | Neodymium ion doped fluoride laser crystal |
CN103275706A (en) * | 2013-05-31 | 2013-09-04 | 湘潭大学 | Blue up-conversion luminescent material and preparation method thereof |
CN107740186A (en) * | 2017-10-30 | 2018-02-27 | 中国科学院上海硅酸盐研究所 | A kind of large scale Yb, R:CaF2/SrF2Laser crystal and preparation method thereof |
CN108559499A (en) * | 2018-05-09 | 2018-09-21 | 长春理工大学 | A kind of bimodulus conversion phosphor |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1203156C (en) * | 2002-12-05 | 2005-05-25 | 苏州大学 | Infrared upward rotating marking material and its prepn. method |
-
2005
- 2005-01-20 CN CNB2005100234734A patent/CN1298895C/en not_active Expired - Fee Related
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008169065A (en) * | 2007-01-10 | 2008-07-24 | Tohoku Univ | Fluoride bulk single crystal material for up-conversion |
CN102534776A (en) * | 2012-03-30 | 2012-07-04 | 中国科学院上海硅酸盐研究所 | Neodymium ion doped fluoride laser crystal |
CN103275706A (en) * | 2013-05-31 | 2013-09-04 | 湘潭大学 | Blue up-conversion luminescent material and preparation method thereof |
CN107740186A (en) * | 2017-10-30 | 2018-02-27 | 中国科学院上海硅酸盐研究所 | A kind of large scale Yb, R:CaF2/SrF2Laser crystal and preparation method thereof |
CN108559499A (en) * | 2018-05-09 | 2018-09-21 | 长春理工大学 | A kind of bimodulus conversion phosphor |
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