CN1030798A - The growing technology of the Yttrium aluminium garnet laser crystal of neodymium-doped and cerium - Google Patents
The growing technology of the Yttrium aluminium garnet laser crystal of neodymium-doped and cerium Download PDFInfo
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- CN1030798A CN1030798A CN88102651A CN88102651A CN1030798A CN 1030798 A CN1030798 A CN 1030798A CN 88102651 A CN88102651 A CN 88102651A CN 88102651 A CN88102651 A CN 88102651A CN 1030798 A CN1030798 A CN 1030798A
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- 239000013078 crystal Substances 0.000 title claims abstract description 73
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 32
- 238000005516 engineering process Methods 0.000 title description 3
- 239000004411 aluminium Substances 0.000 title description 2
- 229910052782 aluminium Inorganic materials 0.000 title description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title description 2
- 239000002223 garnet Substances 0.000 title description 2
- 229910052727 yttrium Inorganic materials 0.000 title description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 230000006698 induction Effects 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 abstract description 65
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 abstract description 3
- -1 cerium yttrium aluminum Chemical compound 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 12
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- 150000002500 ions Chemical class 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 206010070834 Sensitisation Diseases 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
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- 230000008313 sensitization Effects 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000695 excitation spectrum Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The present invention relates to neodymium-doped and cerium yttrium aluminum garnet [(Nd, Ce): YAG] laser crystals draw growth method, comprise aspects such as choosing of growth parameter(s)s such as component, heating means and rotating speed and pulling rate.The present invention has effectively utilized Ce under the condition of not damaging the crystal optics quality
3+→ Nd
3+Energy shift.Make (Nd, Ce): the pulse laser efficiency ratio high-quality neodymium-doped yttrium-aluminum garnet Nd:YAG of YAG improves more than 70%, and it is low to have threshold value, the anti-ultraviolet radiation ability is strong, the repetition rate working stability, stability and cooling to envrionment temperature require advantages such as low, are specially adapted to the medium and small energy pulse laser apparatus of repetition rate work.
Description
The present invention relates to neodymium-doped and cerium yttrium aluminum garnet [(Nd, Ce): YAG] laser crystals draw growth method.
Up to this point (Nd: YAG) monocrystalline remains the laser crystals of excellent property and widespread use.But this crystalline lasing efficiency is not high, and in order to raise the efficiency, many scientific workers have carried out big quantity research.What adopt usually also is that the comparison successful method is at Nd: mix so-called sensitized ions in the YAG crystal.Utilize sensitized ions to Nd
3+Energy shift the utilization ratio that improves pump light source, thereby improve Nd: YAG crystalline lasing efficiency.The best sensitized ions of generally acknowledging is Cr at present
3+, but in the YAG crystal, Cr
3+→ Nd
3+Energy transfer efficiency not high, and transfer time is oversize, so Cr
3+The sensitization effect bad.Particularly in pulse operation, almost there is not positive effect.Seek Nd: the better sensitized ions of YAG crystalline is an important topic in the laser crystals research.
Holloway
(1)Deng observing Ce in the YAG crystal the earliest
3+→ Nd
3+Energy transfer phenomenon.But the just observation of a phenomenon, and the situation of undeclared use sample is not discussed to the mechanism that energy shifts yet.
К О В А Л e В А etc.
(2)In report in 1977, point out, from Nd
3+Fluorescence excitation spectrum see, for two used samples, mix Ce
3+Back Nd
3+Total fluorescence intensity than Nd: the YAG crystal doubles and two times, thereby can come sensitization Nd: YAG with Ce.But the used sample of К О В А Л e В А is the platy-monocrystal of spontaneous crystallization growth in the melt, and the size of monocrystalline does not add explanation.The Nd concentration of its sample be respectively 1.4 and 1.7(wt) %, the concentration of Ce be respectively 0.4 and 0.8(wt) %.Obviously the Nd concentration of the used doping content of К О В А Л e В А in the general laser crystals.
Mares
(3)In its several pieces of reports to the YAG crystal in Ce
3+→ Nd
3+Energy shift and to have carried out careful research.The Nd concentration of specimen in use is 0.96(at) %, the concentration of Ce is 1.4 * 10
-3~2.8 * 10
-2(at) %(calls oneself according to Mares, and specimen in use is provided by Kvapil).Mares points out, has both existed quantity of radiant energy to shift between Ce and Nd, also exists radiationless energy to shift.The efficient that quantity of radiant energy shifts is 14.2%, and radiationless energy shifts and undertaken by dipole-dipole effect and the effect of dipole-four utmost point, since the generation of this process, Ce
3+Fluorescence lifetime drop to two 32~39ns that mix from the 60ns of Ce: YAG.Mares also points out, at low Ce
3+Under the concentration situation, (Ce
3+→ Ce
3+)
n→ Nd
3+The possibility that produces of multistage process little, but Ce
3+When concentration is high, the possibility that produces this multistage process is arranged.But, press Jacobs
(4)Report, Ce may appear when high density
3+Excited state absorption.
Kvapil
(5)Mix Ce and improve Nd Deng once utilizing: the laser activity of YAG.They think, though in the YAG crystal Ce is arranged
3+→ Nd
3+Energy shift, can be used for improving lasing efficiency, but the efficient that energy shifts is not high, and a large amount of Ce mixes to resemble and mixes Cr
3+Equally serious reduction crystalline optical quality.Therefore mix a large amount of Ce
3+Come sensitization Nd
3+Overall utilization benefit not high.Based on this viewpoint, they mix Ce
3+Purpose be not to utilize Ce
3+Sensibilized, but utilize a small amount of Ce
3+Suppress Nd: instantaneous colour center of YAG crystalline and reinforcement inequivalent site Nd
3+Between energy shift, thereby improve lasing efficiency.Kvapil points out, a small amount of Cr
3+Mix, particularly mix a small amount of Ce simultaneously
3+, can suppress the formation of instantaneous colour center effectively, thereby improve continuous laser output, but work as Cr
3+And Ce
3+Concentration be higher than 10
-2(at) during %, the effect that the instantaneous colour center of this inhibition forms weakens and disappears.For pulse laser output, mix the Nd of Ce and Cr: YAG is with (Nd, Ti): YAG is similar.
The Kvapil report (Nd, Ce): the concentration of Nd is 0.6~0.7(wt) % among the YAG, the concentration of Ce is 8 * 10
-4(wt) %, 3 * 10
-3(wt) % and 2 * 10
-2(at) %.In that (Ce): the concentration of Nd and Ce also is like this among the YAG for Nd, Cr.
In (5), there is not detailed report about crystal growth, but from Kvapil
(6)Other work see, their usefulness be the tungsten well heater, growth is drawn by molybdenum pot system.In these reports, equal shapes of undeclared growth interface, but to the choosing and processing of laser bar, their growth interface is protruding in melt.Protective atmosphere during growth is 98% Ar and 2% H
2
From Kvapil
(5)And Mares
(3)Given laser detection data sees, its (Nd, Ce): continuous output and the Nd of YAG: YAG compares not have obviously and improves; And (Ce): the continuous output of YAG is than Nd for Nd, Cr, and YAG improves about 10%.
As mentioned above, at Nd: mix Ce among the YAG and can utilize Ce
3+→ Nd
3+Energy shift and improve lasing efficiency, but then, mix Ce and also can have a strong impact on the crystalline optical quality.Purpose of the present invention be exactly find out a kind of appropriate growth (Nd, Ce): YAG crystalline method, the sensibilized of Ce is fully utilized, can eliminate again or alleviate the infringement of Ce as far as possible optical homogeneity.(Nd, Ce): the YAG crystal becomes laser activity and is better than Nd: YAG and cheap, the practical laser crystals that can extensively promote thereby make.
The present invention be a kind of (Nd, Ce): the YAG laser crystals draw growth method.Comprising the calcination of powder, preparation mixes and moulding, is heated to molten then in crucible and following seed crystal is rotated and draws growth.It is characterized by by chemical formula Y
3-x-yNd
xCe
yAl
5O
12Batching; X=0.0~0.27 wherein, y=5 * 10
-3~0.15; The seed crystal direction is<111 〉,<110〉or<211, crystal diameter compares less than 1/2 with the crucible internal diameter; The crystal rotating speed is 10~150r/min; Pull rate is 0.3~3mm/h; Protective atmosphere is reductibility or neutral atmosphere.
Now details are as follows with the present invention:
As described in document [1-3], in the YAG crystal, Ce is arranged
3+→ Nd
3+Energy shift.К О В А Л e В А
[2]Estimate that from the measuring result of the fluorescence excitation spectrum of Nd for the sample of used melt spontaneous crystallization, the fluorescence intensity of mixing Nd behind the Ce is not for mixing 2~3 times of Ce crystalline.And Mares
[3]Nd from Ce fluorescence
3+Absorption and the structure that produces is estimated Ce
3+→ Nd
3+The quantity of radiant energy transfer efficiency be about 14.2%.Except that the quantity of radiant energy transfer was arranged, Mares pointed out also to have Ce
3+→ Nd
3+Radiationless energy transfer process, even when Ce concentration is high, also have (Ce
3+→ Ce
3+)
n→ Nd
3+The multivalence energy transfer process.Be not difficult to find out in YAG Ce by these results
3+→ Nd
3+The total energy transfer efficiency may with Ce
3+Concentration relevant.On the other hand, as Kvapil
[5]Pointed, a large amount of Ce mixes meeting grievous injury crystalline optical quality, and its one of the main reasons is Ce
3+Ratio of ionic radii Y
3+Greatly, simultaneously also than Nd
3+Greatly, therefore, at Nd: mix a large amount of Ce among the YAG, thereby nature can increase stress infringement crystalline optical quality.In a word, from improving energy transfer efficiency, wish the concentration height of Ce, and, then require the concentration of Ce lower better from the influence of Ce to optical quality.We think that the optimal compromise of energy transfer efficiency and optical quality is and Ce
3+/ Nd
3+Concentration ratio relevant.Therefore, seeking the optimum concn ratio is to make full use of Ce
3+→ Nd
3+Energy shift, can eliminate or alleviate as far as possible the important channel of the harm of Ce again.This also is an important content of the present invention.
As is generally known in the growth, growth parameter(s)s such as crystal rotating speed and pulling rate have a strong impact on crystal mass on drawing.The optimum value of these growth parameter(s)s is then relevant with factors such as melt composition, type of heating, used thermal field, crucible size and crystal diameters.For example, pulling rate is too fast, and can to produce component cold excessively, and crossing then influences crystal mass because the temperature oscillation in the melt is in excessively crystal and too frequent growth-melt back-regrowth state is grown down slowly.For a fixed system, the crystal pulling rate of growth different diameter also should have corresponding adjustment.Therefore, be not difficult to expect the growing system for certain, the melt of different components also should correspondingly be adjusted growth parameter(s).For example, the melt of high Nd concentration and high Ce concentration, pulling rate should suitably slow down.In a word, seeking the optimum growh parameter is another important content of the present invention.
The raw material that uses is preferably high-purity, and the purity of yttrium oxide and Neodymium trioxide is not less than 99.99%, and the purity of aluminum oxide is not less than 99.95% analytical pure, and the purity of cerium oxide is not less than analytical pure, preferably uses spectroscopically pure.Before weighing, all raw materials all need drying to handle.
The raw material that drying is handled is pressed chemical formula Y
3-x-yNd
xCe
yAl
5O
12, the weighing preparation.When definite x and y value, must consider Nd and the segregation coefficient of Ce in YAG, determine the size of x and y by the concentration of Nd and Ce in the segregation coefficient (0.124) of the Nd segregation coefficient (0.15~0.20) of actual measurement or reported in literature and Ce and the desirable crystal.X is generally 0~0.27, and preferred values is 0.09~0.18 concerning concrete use; Y is generally 5 * 10
-3~0.15 even can also be bigger, but from general effect, preferred values is 0.006~0.04.
The raw material that weighs up is through the ground and mixed pre-molding, again through 1100~1600 ℃ of calcinations (also can without calcination).Be noted that in batching, must be strictly on guard against in ground and mixed and the moulding process and sneak into iron and other impurity.
Utilization is generally drawn growing system and is carried out crystal growth.Type of heating can be heated by resistive or induction heating.When using graphite or tungsten electrical resistance heating, the synoptic diagram of its thermal field structure as shown in Figure 1.1 is the molybdenum seed rod among the figure, the 2nd, seed crystal, the 3rd, crystal, the 4th, melt, 5, the 6, the 7th, heat protection screen on the molybdenum, the 8th, molybdenum crucible, the 9th, the holder of molybdenum pot, the 10,11, the 12nd, molybdenum side heat protection screen, the 13rd, inner shield tube, the 14th, resistance heater, the 15th, pallet, the 16th, battery lead plate, the 17th, molybdenum platform cover, the 18th, web member, the 19th, aluminum oxide pad.
When using induction heating, the synoptic diagram of its thermal field structure as shown in Figure 2.1 is vision slit among the figure, the 2nd, and the crystal pulling hole, the 3rd, seed rod, the 4th, seed crystal, the 5th, the zirconium dioxide stay-warm case, the 6th, crystal, the 7th, melt, the 8th, the iridium crucible, the 9th, ruhmkorff coil, the 10th, the zirconium dioxide insulation is husky, and the 11st, ceramic heat-preservation cylinder, the 12nd, pallet.
It is molten to place crucible slowly to be heated to the raw material of pre-molding.When utilizing resistive heating, use molybdenum or tungsten crucible; When utilizing induction heating, use the iridium crucible.After treating that raw material fully melts, seed crystal gradually descends.The seed crystal direction is<111 〉, also can use<110,<211〉or the seed crystal of other direction, but preferably<111 ± 5 ° seed crystal.After treating that seed crystal contact melt is also stable, the beginning pulling growth.In following seed crystal process, melt temperature needs suitably to adjust.In initial period of growth with generally to draw growth the same, need are through receipts neck and shouldering process.After changing isodiametric growth over to, the crystalline diameter should control to less than 1/2 of crucible interior diameter, is generally 1/2.5~1/4, is preferably in 1/3~1/3.5 scope.
As is generally known draw growth of Nd: during the YAG crystal, whether proper growth parameter(s)s such as rotating speed and pulling rate selected for use, and the crystalline performance is had a significant impact.Because Ce
3+Ratio of ionic radii Nd
3+And Y
3+All big, therefore, (Nd, Ce): during YAG, selecting for use of growth parameter(s) is even more important in growth.For example, the size of rotating speed and stability thereof all have a significant impact the shape and the optical homogeneity of crystal growth interface.Rotating speed used in the present invention by the selection of rotating speed, can make crystal growth with protruding protruding interface growth to melt in 10~150r/min scope; Also can plane interface growth.When selecting protruding interface growth for use, rotating speed generally is lower than 45r/min, as is heated by resistive, and its preferred values is 10~30r/min; Use induction heating, its preferred values is 10~40r/min.When selecting plane interface growth for use, the preferable rotating speed of resistive heating is 50~120r/min, and the preferable rotating speed of induction heating is 50~100r/min.As for the optimal values of rotating speed, not only relevant with the shape of growth interface, and also relevant with crucible size and crystal diameter.In general, crystal diameter is big with the ratio of crucible diameter, and rotating speed should hang down; The little rotating speed of ratio should be high.The stability that is noted that rotating speed also is an important factor, and particularly during plane interface growth, the instantaneous fluctuating of rotating speed must not surpass ± 0.5r/min.
Pull rate is another important growth parameter(s).Pulling rate is crossed conference and is produced that component is cold excessively to scrap crystal, and the too small crystal that may make of pulling rate is grown in too frequent growth-melt back-regrowth process, can increase the weight of striation stress.Selecting for use of pulling rate should be according to employed thermal field situation, doping content, the decision of factors such as interface shape and crystalline diameter.The used pulling rate scope of the present invention is 0.3~3.0mm/h, and when protruding interface growth, the preferable pulling rate of resistive heating is 0.8~1.4mm/h, and the preferable pulling rate of induction heating is 0.5~1.2mm/h.When plane interface growth, the preferable pulling rate of resistive heating is 1.1~2.2mm/h, and the preferable pulling rate of induction heating is 0.6~1.5mm/h.In general, the crystalline diameter is big or doping content is high, and pulling rate should be slow; Otherwise pulling rate can suitably add piece.
Another need specify the protective atmosphere when being growth.Owing to mix Ce, the Ce ion may be a trivalent, also may be tetravalence, and the tetravalence attitude is more stable.That have sensibilized is trivalent Ce, therefore, the protective atmosphere during growth should be a neutral, but reductibility preferably.The protective atmosphere that the present invention uses is that purity is the Ar of 4N, also available N
2Or Ar+H
2And Ar+N
2
On drawing the growth in, temperature controlled importance is that everybody knows, the present invention require temperature-controlled precision be not less than ± 0.5 ℃.
Example 1.
Press chemical formula Y
3-x-yNd
xCe
yAl
5O
12Match raw material, x=0.12 wherein, y=0.06.The raw material gross weight is 300 grams.Confected materials places the agate alms bowl to mix 1 hour, in the special latex rubber bag of packing into then (shared four layers), places pre-molding in the oil press.The material piece that suppresses places the crucible shown in the accompanying drawing 1, and crucible is φ 60 * 30mm crucible that molybdenum sheet is stamped to form, closed furnace door, and by common growth of Nd: YAG crystalline method vacuumizes, and fills Ar gas.Utilize graphite resistance heating unit (as 14 in the accompanying drawing 1) slowly to be heated to fusing fully.Fall seed crystal gradually, the seed crystal direction is<111〉± 5 °.When seed crystal drops to liquid level, need to adjust melt temperature and make it be suitable for drawing growth.After treating seed crystal contact melt, stablized 1 hour, begin pulling growth then.
In process of growth, rotating speed is 80r/min, and pulling rate is 2mm/h.The diameter of equal-diameter part is controlled to be 20~23mm.Temperature-controlled precision is not less than ± and 0.5 ℃.
When finishing growth, manually mention crystal and make it just break away from liquid level.Stop then lifting and slowly cooling, reduce to 600 ℃ with 10 hours time, outage is chilled to room temperature with stove, thus the end whole growth process.
Example 2
The preparation of raw material is identical with example 1 with process of growth, and different is that rotating speed is 15r/min, and pulling rate is 1.2mm/h.
Material component in other example, type of heating, crucible situation and growth parameter(s) are all listed in the table 1.Other process and method is identical with example 1 or example 2.
The growth of application the technology of the present invention (Nd, Ce): the YAG crystal, can utilize Ce fully
3+→ Nd
3+Energy transfer phenomenon, and avoid or weakened Ce
3+Influence to the crystal optics quality.Avoid φ 3~φ 6 of being processed in the facet growth district laser bar extinction ratio greater than 25dB surpass 90%, and wherein the overwhelming majority surpasses 30dB.Only there is the extinction ratio of only a few laser bar to be lower than 20dB (and this is owing to do not avoid fully due to the facet district).Except at light
Learn the homogeneity aspect and can satisfy fully outside practical the requirement, the present invention's growth (Nd, Ce): the YAG crystal also has the following advantages:
(Nd, Ce): YAG crystalline lasing efficiency height.Just the result who has reached sees, when 10 joules of inputs, comparable 1986 national Nd of its static efficiency: the prize-winning rod of YAG crystal system amount comparation and assessment is high more than 70%, and doubles approximately when importing 5~6 joules.Accompanying drawing 3 is part (Nd, Ce): the static pulse output of YAG crystalline and 86 years prize-winning Nd:YAG(comparation and assessment numbering H510 of national qulity appraisal) contrasts under same test condition.The laser pump cavity that test is used for oval (2a=24,2b=21mm), the long 70mm in chamber, xenon lamp are φ 5.3 * 60mm, the outgoing mirror reflectivity is 45%, the energy of use is counted U.S. Boulder company 365 types.Curve 1~5th in the accompanying drawing 3, (Nd, Ce): the static pulse curve of output of YAG.The size 1~3rd of laser bar, φ 5 * 80mm, the 4th, φ 5 * 65mm, the 5th, φ 4 * 50mm.Curve 6 is national Nd in 1986: the Nd that the YAG qulity appraisal is prize-winning: the curve of output of YAG (comparation and assessment are numbered H510), rod is of a size of φ 5 * 76mm.As seen from the figure, curve 1 and 2 higher more than 70% than 6 output 10 joules of whens input.
(Nd, Ce): YAG crystalline laser threshold is lower than present high-quality Nd significantly: the YAG rod.Can see that from accompanying drawing 3 (Nd, Ce): YAG crystalline laser threshold has reduced by 0.5~1.0 joule.
(Nd, Ce): the YAG crystal has stronger uvioresistant irradiation ability.Utilize this crystalline laser apparatus not need to filter the ultraviolet measure.Device has been simplified in the pollution that this characteristic has not only avoided filter liquor etc. to bring, and near the ultraviolet luminous energy the 340nm of light source is effectively utilized.
(Nd, Ce): the YAG crystal does not have common Nd: YAG crystalline output attenuation phenomenon.We work long hours continuously with per 5 seconds repetition rates once under 19.2 joules input, and the energy of its each output is stable.And Nd: the YAG crystal often has and significantly reduces phenomenon gradually, can reduce more than 20% when serious.
(Nd, Ce): the characteristic of YAG crystal under repetition rate work obviously is better than Nd: the YAG crystal.Under simple air-cooled condition, (Nd, Ce): the speed that the output of YAG crystalline pulse laser descends with repetition rate is considerably slower than Nd: the YAG crystal.Table 2 be (Nd, Ce): YAG crystal and the prize-winning rod of 86 years national Nd: YAG rod qulity appraisal are exported energy under different repetition rates comparison.
Table 2.(Nd, Ce): YAG rod and Nd: YAG is laser output contrast under repetition rate
Sample | Size |
2 times/second | 5 times/second | 10 times/second | ||
(Nd,Ce):YAG | φ5×80mm | 235mj | 234mj | 198mj |
Nd; YAG comparation and assessment numbering H510 | φ5×76mm | 135mj | 125mj | 105mj |
(Nd, Ce): the stability of envrionment temperature is strong during the output of YAG crystal laser.Forcing under the closed air-cooled condition, repetition rate work with 10 times/second, when envrionment temperature when 30 ℃ rise to 100 ℃, (Nd, Ce): YAG crystalline laser output energy only descends 5~6%, and (more than 10 minutes) work for a long time, still can works better when envrionment temperature is raised to 150 ℃.And Nd: YAG did not just almost have laser output after working 90 seconds in 50 ℃ environment under same working conditions.
Reference
[1]W.W.Holloway et.al.,J.Opt.Soc.Am.V59,60,(1969)
[2]Н.С.Ковалева и.др.,Ж.Прик、Спект.Т27,546(1977)
[3]J.A.Marěs;Czech,J.Phyz.B35 883(1985);
B36,1079(1986);
Rev.Phyz.Appl,V22,145,(1987)
[4]R.R.Jacobs et.al.,Appl.Phyz.Lett.V33,410(1978)
[5]J.Kvapil et.al.,Czech.J.Phyz.B34 581(1984)
B.Perner et.al., Czech patents, 240641
[6]J.Kvapil et.al.,ibid.B29 1282(1979)
[7]J.Kvapil et.al.,ibid.B23 817(1982)
Claims (10)
1, a kind of (Nd, Ce): the YAG laser crystals draw growth method, comprising calcination, preparation, mixing and the moulding of powder, in crucible, be heated to molten and following seed crystal then, be rotated and draw growth.It is characterized by by chemical formula Y
3-x-yNd
xCe
yAl
5O
12Batching, x=0~0.27 wherein, y=5 * 10
-3~0.15; The seed crystal direction is<111 〉,<110 or<211; Crystal diameter compares less than 1/2 with the crucible interior diameter; The crystal rotating speed is 10~150r/min, and pulling rate is 0.3~3mm/h; Protective atmosphere is reductibility or neutral atmosphere.
2, according to the described method of claim 1, it is characterized by chemical formula Y
3-x-yNd
xCe
yAl
5O
12Middle x=0.09~0.18, y=0.006~0.04; Nd concentration is 0.6(at in the crystal) % of %~1.2(at), the concentration of Ce is 2.5 * 10
-2(at) % of %~0.16(at).
3, according to claim 1 or 2 described methods, adopt graphite resistance heating and molybdenum crucible, to grow with protruding interface, rotating speed is 10~40r/min, pull rate is 0.8~1.4mm/h.
4, according to the described method of claim 3, grow with planar interface, rotating speed is 50~120r/min, and pull rate is 1.0~2.2mm/h.
5, according to claim 1 or 2 described methods, adopt induction heating and iridium crucible, and grow with protruding interface, rotating speed is 10~40r/min, pull rate is 0.5~1.5mm/h.
6, according to the described method of claim 5, grow with planar interface, rotating speed is 50~100r/min, and pull rate is 0.6~1.5mm/h.
7, according to claim 1 or 2 described methods, adopt tungsten resistive heating and molybdenum crucible or tungsten crucible, to grow with protruding interface, rotating speed is 10~40r/min, pull rate is 0.8~1.4mm/h.
8, according to the described method of claim 7, grow with planar interface, rotating speed is 60~120r/min, pull rate 1.0~2.2mm/h.
9, according to the described method of above-mentioned each claim, wherein the seed crystal direction is<111〉± 5 °,<110〉± 5 ° or<211 ± 5 °.
10, according to the described method of above-mentioned each claim, wherein powder fully grinds evenly, and batching is preceding 1000~1350 ℃ of following calcinations 2~8 hours.
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CN101338453B (en) * | 2008-07-16 | 2011-02-16 | 成都东骏激光股份有限公司 | Growth method of large size non-core YAG series laser crystal |
CN102362399A (en) * | 2009-03-23 | 2012-02-22 | 皇家飞利浦电子股份有限公司 | Optically pumped solid-state laser and lighting system comprising said solid-state laser |
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CN103469298A (en) * | 2013-08-22 | 2013-12-25 | 昆山开威电子有限公司 | Growth method of cerium-doped yttrium aluminium garnet single crystal by adopting kyropoulos method and high-temperature furnace |
CN104746135A (en) * | 2013-12-27 | 2015-07-01 | 成都晶九科技有限公司 | Growth method of induction furnace planar-interface large-sized neodymium-doped yttrium aluminium garnet crystal |
CN104746135B (en) * | 2013-12-27 | 2017-04-19 | 成都晶九科技有限公司 | Growth method of induction furnace planar-interface large-sized neodymium-doped yttrium aluminium garnet crystal |
CN104313693A (en) * | 2014-09-19 | 2015-01-28 | 北京雷生强式科技有限责任公司 | Yttrium aluminum garnet laser crystal doped growth device, crystal growth furnace and preparation method thereof |
CN104313693B (en) * | 2014-09-19 | 2017-01-18 | 北京雷生强式科技有限责任公司 | Yttrium aluminum garnet laser crystal doped growth device, crystal growth furnace and preparation method thereof |
CN106087056A (en) * | 2016-08-03 | 2016-11-09 | 成都新源汇博光电科技有限公司 | A kind of growth technique for YAG crystal |
CN106087056B (en) * | 2016-08-03 | 2019-02-01 | 成都新源汇博光电科技有限公司 | A kind of growth technique for YAG crystal |
CN110453284A (en) * | 2018-05-08 | 2019-11-15 | 安徽科瑞思创晶体材料有限责任公司 | A kind of GAGG scintillation crystal manufacturing method |
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