CN102691104A - Ytterbium-doped gadolinium yttrium aluminum garnet crystal and growth method thereof - Google Patents
Ytterbium-doped gadolinium yttrium aluminum garnet crystal and growth method thereof Download PDFInfo
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- CN102691104A CN102691104A CN2012102084074A CN201210208407A CN102691104A CN 102691104 A CN102691104 A CN 102691104A CN 2012102084074 A CN2012102084074 A CN 2012102084074A CN 201210208407 A CN201210208407 A CN 201210208407A CN 102691104 A CN102691104 A CN 102691104A
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Abstract
The invention provides an ytterbium-doped gadolinium yttrium aluminum garnet crystal and a growth method thereof, and belongs to the technical field of photoelectron materials. The existing Yb:Y3Al5O12 crystal is low in doping concentration and low in doping uniformity and has less possibility of achieving high-power laser output when serving as a laser material. According to the existing Yb:Y3Al5O12 crystal growth method, the Yb:Y3Al5O12 has a high smelting point of 1,950 DEG C, so that the volatilization amount of yttrium in an yttrium crucible is large, the side effect is high, the quality of the crystal is poor, and the size is small. The molecular formula of the ytterbium-doped gadolinium yttrium aluminum garnet crystal is Yb:Y2GdAl5O12, and the crystal base is yttrium aluminum garnet. According to the growth method of the ytterbium-doped gadolinium yttrium aluminum garnet crystal, the growth material comprises yttrium oxide (Y2O3), gadolinium oxide (Gd2O3) and aluminum oxide (Al2O3) at a chemical metering ratio of 2:1:5; after x moles of ytterbium oxide is added into the growth material, the adding amount of the Gd2O2 is required to be reduced by (1-x) mole on the basis of the chemical metering ratio; and the growth process parameters of the crystal are determined as follows: the pull speed is between 0.5 and 0.8 mm/h, the rotation speed is between 12 and 18 rpm and the growth temperature is 1,880 DEG C.
Description
Technical field
The present invention relates to a kind of ytterbium yttrium yttrium aluminmiu garnet crystal and growth method thereof of mixing, mixing ytterbium yttrium yttrium aluminmiu garnet crystal is a kind of laser crystals, and molecular formula is Yb:Y
2GdAl
5O
12, belong to the photoelectron material technical field.
Background technology
Mix the ytterbium laser applications in fields such as laser processing, laser display, laser medicine, environment measuring, communication, information processing, scientific researches.In addition, mixing ytterbium laser has absorption more by force in water, thus not only to eye-safe, and can accurately get involved biological tissue, therefore, also can be applied to medical fields such as ophthalmologic operation.
Mix the used laserable material of ytterbium laser for mixing the ytterbium crystal, comprise oxide crystal, like Yb:Y
3Al
5O
12, belonging to isometric system, crystal substrate is a yttrium aluminum garnet, its absorption and emission peak are comparatively approaching, have advantages such as the bandwidth of absorption, fluorescence lifetime length, accurate four-level structure.But, because ytterbium, ruthenium ion radius matching degree are low, so doping content is low, the doping content of ytterbium is the highest has only 30at.%, and uniform doping property is also poor, thereby, be difficult to obtain high power laser output as laserable material.
Existing Yb:Y
3Al
5O
12The crystalline growth method is following:
1, growth material preparation
Be the crystal of acquisition lattice perfection, the binding crystal growthing process parameter, the stoichiometric ratio of confirming growth material component yttrium oxide, aluminum oxide is Y
2O
3: A1
2O
3=3:5.In view of the above, the proportioning of each component is following in the growth material: Yb
2O
3Be x mole, Y
2O
3Be (1-x) mole, Al
2O
3Be 5 moles, wherein the span of x is: 0.005mol≤x≤0.30mol.With said three component thorough mixing, get block growth material with the hydropress briquetting.
2, crystal growth
Adopt Czochralski grown Yb:Y
3Al
5O
12Crystal.With the prepared block growth material single crystal growing furnace of packing into, vacuumize, charge into nitrogen, the main technologic parameters of crystal growth is confirmed as: pull rate 0.6 ~ 0.8mm/h, speed of rotation 12 ~ 16rpm, 1950 ℃ of growth temperatures.
3, annealing
After crystal growth finishes, adopt the mode of in-situ annealing slowly furnace temperature to be reduced to room temperature, take out crystal.
Said growing method also has its deficiency, at growth Yb:Y
3Al
5O
12In the crystalline process, because Yb:Y
3Al
5O
12Fusing point is high, and as 1950 ℃, thereby the iridium volatile quantity in the iridium crucible is big, and its negative effect comprises: 1, evaporable iridium gets into melt, becomes detrimental impurity; 2, get into furnace chamber atmosphere, block viewing window; 3, invest crystal growing surface, stop the crystalline growth, cause slow, the cracking of crystal growth.Under the influence of these negative effects, be difficult to grow high quality, large-sized Yb:Y
3Al
5O
12Crystal has only Φ 20mm * 50mm like crystalline size.
Summary of the invention
In order to improve the doping content of mixing the ytterbium oxide crystal, and can grow large-sized crystal, we propose a kind of scheme of mixing ytterbium yttrium yttrium aluminmiu garnet crystal and growth method thereof.
The present invention's the ytterbium yttrium yttrium aluminmiu garnet crystal of mixing belongs to isometric system, and the REE ytterbium is a dopant ion, it is characterized in that, said to mix ytterbium yttrium yttrium aluminmiu garnet crystal molecule formula be Yb:Y
2GdAl
5O
12, crystal substrate is the yttrium yttrium aluminmiu garnet.
The present invention's its step of ytterbium yttrium yttrium aluminmiu garnet growing method of mixing comprises growth material preparation, crystal growth and annealing; The growth material component comprises ytterbium oxide, yttrium oxide, aluminum oxide; It is characterized in that; The growth material component also comprises gadolinium sesquioxide, and yttrium oxide, gadolinium sesquioxide, aluminum oxide stoichiometric ratio are Y
2O
3: Gd
2O
3: Al
2O
3=2:1:5, after confirming to add x mole ytterbium oxide, Gd
2O
3Add-on need on the basis of said stoichiometric ratio, reduce (1-x) mole, the crystal growth technique parameter is confirmed as: pull rate 0.5 ~ 0.8mm/h, speed of rotation 12 ~ 18rpm, 1880 ℃ of growth temperatures.
Its effect of the present invention is Yb:Y
2GdAl
5O
12Crystal belongs to isometric system and zero defect; Because ytterbium, gadolinium ion radius matching degree height; Make the ytterbium doping content reach as high as 100at.%, the raising of uniform doping property, thereby for confirming that as required doping content created prerequisite; This highly doped effect can be that the present invention's the peak value of mixing the ytterbium yttrium yttrium aluminmiu garnet crystallofluorescence spectrogram is found out from accompanying drawing, and curve 1, curve 2 are respectively existing Yb:Y among the figure
3Al
5O
12Crystal, the present invention's Yb:Y
2GdAl
5O
12Crystallofluorescence spectrogram, latter's fluorescence intensity peak value are apparently higher than the former, and still, the fluorescence spectrum of the two is similar, the photoluminescence peak wavelength is close.Aspect method, Y
2GdAl
5O
12Crystalline melting point has only 1880 ℃, is starkly lower than existing Yb:Y
3Al
5O
12The fusing point that crystal is 1950 ℃, consistent with it crystal growth temperature obviously reduces, and the iraurite volatile quantity reduces, thereby can easily grow high quality, large-sized crystal, like Φ 40mm * 60 ~ 80mm, satisfies the needs of great-power solid laser
Description of drawings
Accompanying drawing be the present invention mix ytterbium yttrium yttrium aluminmiu garnet crystallofluorescence spectrogram, this figure is simultaneously as Figure of abstract.
Embodiment
The present invention's the ytterbium yttrium yttrium aluminmiu garnet crystal of mixing belongs to isometric system, and the REE ytterbium is a dopant ion, and said to mix ytterbium yttrium yttrium aluminmiu garnet crystal molecule formula be Yb:Y
2GdAl
5O
12, crystal substrate is the yttrium yttrium aluminmiu garnet, the concentration of mixing of ytterbium is 10 ~ 100at.%.
The present invention to mix ytterbium yttrium yttrium aluminmiu garnet growing method particular content following:
1, growth material preparation
Growth material component yttrium oxide, gadolinium sesquioxide, aluminum oxide are by stoichiometric ratio Y
2O
3: Gd
2O
3: Al
2O
3=2:1:5 adds, and each set of dispense that comprises ytterbium oxide is such as descending Yb
2O
3Be x mole, Gd
2O
3Be (1-x) mole, Y
2O
3Be 2 moles, Al
2O
3Be 5 moles, wherein the span of x is: 0.005mol≤x≤1mol.With said four component thorough mixing, adopt the solid phase method sintering, get block growth material with the hydropress briquetting.
2, crystal growth
Adopt Czochralski grown Yb:Y
2GdAl
5O
12Crystal.With the prepared block growth material single crystal growing furnace of packing into, vacuumize, charge into nitrogen, the main technologic parameters of crystal growth is confirmed as: pull rate 0.5 ~ 0.8mm/h, speed of rotation 12～18rpm, 1880 ℃ of growth temperatures.
3, annealing
Crystal growth finishes, and adopts the mode of in-situ annealing slowly furnace temperature to be reduced to room temperature, takes out crystal.
Illustrate the present invention below.
Growth material component yttrium oxide, gadolinium sesquioxide, aluminum oxide are by stoichiometric ratio Y
2O
3: Gd
2O
3: Al
2O
3=2:1:5 adds.Get x=0.1, the proportioning of each component is following in the growth material, Yb
2O
3Be 0.1 mole, Gd
2O
3Be 0.9 mole, Y
2O
3Be 2 moles, Al
2O
3It is 5 moles.With said four component thorough mixing, adopt the solid phase method sintering, get block growth material with the hydropress briquetting.Adopt Czochralski grown Yb:Y
2GdAl
5O
12Crystal.With pack into iridium crucible and put into the Frequency Induction Heating single crystal growing furnace of prepared block growth material, be evacuated to 10-4Pa, charge into nitrogen.The main technologic parameters of crystal growth is confirmed as: pull rate 0.6mm/h, speed of rotation 14rpm, 1880 ℃ of growth temperatures.Crystal growth finishes, and adopts the mode of in-situ annealing slowly furnace temperature to be reduced to room temperature, takes out crystal.This crystal belongs to isometric system for mixing ytterbium yttrium yttrium aluminmiu garnet crystal, and crystal mass is better, is of a size of Φ 40mm * 63mm.Through test, the concentration of mixing of ytterbium is 10at.%.Through the fluorescence spectrum test, the present invention's the ytterbium yttrium yttrium aluminmiu garnet crystal of mixing is compared with existing yttrium aluminum garnet crystal with ytterbium doping, and fluorescence spectrum is similar; The photoluminescence peak wavelength is close; The concentration of mixing of ytterbium is all 10at.%, and photoluminescence peak but has raising, sees shown in the accompanying drawing; Can know, the present invention mix the crystal doping of ytterbium yttrium yttrium aluminmiu garnet evenly, the crystal growth quality is high.
Claims (4)
1. mix ytterbium yttrium yttrium aluminmiu garnet crystal for one kind, belong to isometric system, the REE ytterbium is a dopant ion, it is characterized in that, said to mix ytterbium yttrium yttrium aluminmiu garnet crystal molecule formula be Yb:Y
2GdAl
5O
12, crystal substrate is the yttrium yttrium aluminmiu garnet.
2. the ytterbium yttrium yttrium aluminmiu garnet crystal of mixing according to claim 1 is characterized in that the concentration of mixing of ytterbium is 10 ~ 100at.%.
3. mix ytterbium yttrium yttrium aluminmiu garnet growing method for one kind; Its step comprises growth material preparation, crystal growth and annealing; The growth material component comprises ytterbium oxide, yttrium oxide, aluminum oxide; It is characterized in that the growth material component also comprises gadolinium sesquioxide, yttrium oxide, gadolinium sesquioxide, aluminum oxide stoichiometric ratio are Y
2O
3: Gd
2O
3: Al
2O
3=2:1:5, after confirming to add x mole ytterbium oxide, Gd
2O
3Add-on need on the basis of said stoichiometric ratio, reduce (1-x) mole, the crystal growth technique parameter is confirmed as: pull rate 0.5 ~ 0.8mm/h, speed of rotation 12 ~ 18rpm, 1880 ℃ of growth temperatures.
4. the ytterbium yttrium yttrium aluminmiu garnet growing method of mixing according to claim 3 is characterized in that, growth material comprises each set of dispense of ytterbium oxide such as following, Yb
2O
3Be x mole, Gd
2O
3Be (1-x) mole, Y
2O
3Be 2 moles, Al
2O
3Be 5 moles, wherein the span of x is: 0.005mol≤x≤1mol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297136A (en) * | 2015-11-13 | 2016-02-03 | 孙雷 | Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof |
| CN108085743A (en) * | 2017-12-25 | 2018-05-29 | 吉林建筑大学 | Mix ytterbium lutetium yttrium yttrium aluminmiu garnet crystal and preparation method thereof |
| CN108866627A (en) * | 2018-07-16 | 2018-11-23 | 苏州四海常晶光电材料有限公司 | A kind of neodymium erbium is co-doped with GYAG laser crystal and preparation method thereof |
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| 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 growth method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105297136A (en) * | 2015-11-13 | 2016-02-03 | 孙雷 | Cerium-doped gadolinium lutecium aluminate garnet crystal for laser illumination and preparation method thereof |
| CN108085743A (en) * | 2017-12-25 | 2018-05-29 | 吉林建筑大学 | Mix ytterbium lutetium yttrium yttrium aluminmiu garnet crystal and preparation method thereof |
| CN108866627A (en) * | 2018-07-16 | 2018-11-23 | 苏州四海常晶光电材料有限公司 | A kind of neodymium erbium is co-doped with GYAG laser crystal and preparation method thereof |
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Application publication date: 20120926 |