CN101871125A - High-temperature rare earth oxide laser crystal and preparation method thereof - Google Patents
High-temperature rare earth oxide laser crystal and preparation method thereof Download PDFInfo
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- CN101871125A CN101871125A CN 201010190075 CN201010190075A CN101871125A CN 101871125 A CN101871125 A CN 101871125A CN 201010190075 CN201010190075 CN 201010190075 CN 201010190075 A CN201010190075 A CN 201010190075A CN 101871125 A CN101871125 A CN 101871125A
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Abstract
The invention relates to a rare earth oxide crystal and a preparation method thereof. The structural general formula of the crystal is (LnxRe1-x)2O3, the crystal belongs to a cubic crystal system, the space group is Ia3, and the crystal is in a bixbyite structure. The preparation method of the rare earth oxide laser crystal comprises the following steps of: firstly, manufacturing polycrystalline materials by taking Re2O3 and Ln2O3 as raw materials; then, manufacturing material bars; and filling the material bars into an optical floating zone growing furnace for growing according to a floating zone method. The method of the invention has high speed and short cycle, a crucible is not needed in crystal growth, the pollution on the crystal is reduced, and the growing crystal has high transparency and less cracks and is suitable for laser devices.
Description
Technical field
The present invention relates to a series of high-temperature rare earth oxide crystal and preparation method thereof, belong to the high-temperature oxide field of laser crystal materials.
Background technology
Since the sixties in last century, research has caused the great interest of people because the rare earth oxide crystal has fabulous thermomechanical property to the rare earth oxide crystalline, for example: high heat conductance, the good optical characteristic comprises low phonon energy and wide perviousness (from the visible light to the region of ultra-red), make them can be used as laser host material. for laser crystals, thermal conductivity and crystalline light injury threshold have confidential relation, big thermal conductivity can improve the crystalline light injury threshold, improve pump power, thereby the raising output rating, so active ions Doped Rare Earth oxide crystal can be used for superpower output.Except having high thermal conductivity, the rare earth oxide crystal multiple active ions that can mix comprise transition metal ion, thereby can produce the laser of many wave bands.Have lot of advantages just because of the rare earth oxide crystal, people more and more pay close attention to the research of adulterated pottery of active ions or crystalline performance.But the fusing point of these rare earth oxides is especially high, and (more than 2400 ℃) are so that grow their method difficult and complexity.Up to the present, this crystal-like method of the growth of being reported has molten flame method, crystal pulling method, heat-exchanging method, laser heated pedestal method, Bridgman method, falling crucible method and electrochemical method.But these methods have the shortcoming of oneself, and czochralski method and heat-exchanging method need to use the rhenium crucible, cause easily the pollution of crystal.And molten flame method and electrochemical method growth are difficult to obtain the monocrystalline of satisfactory bulk, and growth is second-rate.So seek out the bulky single crystal of high optical quality, need to seek other suitable growth methods.The light float-zone method has the incomparable advantage of above-mentioned additive method: do not use crucible, can not cause crucible that crystalline is polluted; Can under oxygen atmosphere, grow, can remedy the oxygen defect that growth forms under nitrogen atmosphere; Have the higher speed of growth, growth cycle is short, can obtain oxide monocrystal fast.Experimental result shows: at Wen Chang, can adopt the optics float-zone method to grow centimetre-sized under the situation that growth velocity is controlled well, high quality rare earth oxide crystal, and crystal physicochemistry excellent performance.Referring to document: H.Tsuiki, K.Kitazawa, T.Masumoto, K.Shiroki_and K.Fueki, J.crystal Growth, 49 (1980) 71-76, these advantages of rare earth oxide laser crystal make it can become excellent laser host.At present, adopt the rare earth oxide laser crystal of floating zone method growth as gain medium, report is not yet arranged.
Summary of the invention
Complicated and difficult for present rare earth oxide crystal technique the invention provides grow the efficiently method of rare earth oxide crystal of a kind of economy.
The general formula of rare earth oxide crystal of the present invention is (Ln
xRe
1-x)
2O
3This crystalloid has high optical quality and high thermal conductivity, is good gain medium.
Technical scheme of the present invention is as follows:
One, rare earth oxide laser crystal (Ln
xRe
1-x)
2O
3
Rare earth oxide series laser crystal general structure of the present invention is: (Ln
xRe
1-x)
2O
3, 0＜x＜0.3.
Wherein, Ln=Yb, Nd, Tm, Er, Ho, Yb
yEr
1-yOr Tm
yHo
1-y0＜y＜1;
Re=Lu, Sc, Lu
zY
1-zOr Sc
zY
1-z0＜z＜1.
(Ln of the present invention
xRe
1-x)
2O
3Crystal is cubic system, and space group is Ia3, the bixbyite structure.
Preferably, work as Ln=Nd, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.05
Preferably, work as Ln=Yb, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.3
Preferably, work as Ln=Er, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.03
Above-mentioned have a general formula (Ln
xRe
1-x)
2O
3Crystal, fusing point is all very high, wherein the most representatively is:
(Nd
xLu
1-x)
2O
3, x=0.01, unit cell parameters:
Fusing point: 2510 ℃,
(Ln
xSc
1-x)
2O
3, x=0.01, unit cell parameters:
Fusing point: 2450 ℃.
Two, (Ln
xRe
1-x)
2O
3The crystalline preparation method
(Ln of the present invention
xRe
1-x)
2O
3The preparation method of crystal is with Re
2O
3And Ln
2O
3Be raw material, adopt the floating zone method growth, used grower is optics float zone growth stove, adopts four xenon lamp heating, and crystal growth step comprises:
(1) according to (Ln
xRe
1-x)
2O
3The molar ratio weighing raw material of each component and mixing in the formula is put into the Pt crucible at 1000～1100 ℃ of sintering, and insulation 8h gets polycrystal material, and is for subsequent use.
(2) with agate mortar polycrystal is ground, be milled into fine powder, median size 4 μ m get 20-30g and 15-20g material respectively and pack in two balloons; Vacuumize after installing,, make two poles that diameter is identical, length is different 68KN hydrostatic compacting 1-1.5 minute, and then in whirl-sintering furnace 1500 ℃ burnt 4-5 hour, polycrystalline rod;
(3) in optics float zone growth stove, fix long and short two polycrystalline rods on the position of upper and lower charge bar bar respectively, a wherein following polycrystalline rod is the seed crystal rod, above a polycrystalline rod be charge bar, with silica tube seed crystal rod and charge bar are sealed, the program of setting by the float zone growth stove was warming up to 2500 ℃ with 4-4.5 hour, make as the upper end of seed crystal rod and the charge bar lower end fusing of its top and contact, the control growing temperature range is 2400-2500 ℃, set the pull rate and the rotating speed of crystal growth, the beginning crystal growth.
(4) crystal growth finishes, and slowly reduces to room temperature through 5-5.5 hour, and crystal is come out of the stove; The crystal of the coming out of the stove 30-32h that anneals under 1500 ℃ temperature, annealing atmosphere is an atmosphere.
Preferably, two pole diameters of compacting are 8-10mm in the above-mentioned steps (2), and the length of long rod is 60-80mm, and the length of stub is 30-40mm.The length of preferred long rod is 2 times of stub length.
Further preferred, two diameter of the rods of compacting are 10mm in the above-mentioned steps (2), and length is respectively 80mm, 40mm.
The pull rate of crystal growth is 5-8mm/h in the above-mentioned steps (3), rotating speed 20-30r/min.
In the above-mentioned steps (3), preferred crystal growth is carried out under the oxygen protective atmosphere, and oxygen purity is 99.9%, and the oxygen ventilation amount is 50mL/min.
More than said crystal processed, polished, all adopt state of the art to get final product.
More than said optics float zone growth stove adopt four xenon lamps heating, top temperature can reach 3000 ℃.
More than the setting of said intensification, cooling and crystal pull rate and the rotating speed specification of all consulting optics float zone growth stove carry out.The present invention does not add the part of detailed description and is all undertaken by the specification sheets of optics float zone growth stove.
The present invention utilizes the float-zone method growing crystal, can obtain a centimetre magnitude, high-quality rare earth oxide crystalline material within a short period of time.
Rare earth oxide growing method speed of the present invention is fast, and the cycle is short, and crystal growth does not need crucible, reduces crystalline is polluted, and is better than other growth method.The crystal of being grown has high transparent, and it is less to ftracture, and is suitable as laserable material, is used to make Laser Devices
Description of drawings
Fig. 1 is a crystal growing apparatus synoptic diagram of the present invention, wherein: 1, unloading rod bar (seed rod), 1 ', loading rod bar (raw material bar), 2, inlet mouth, 3, the seed crystal rod, 4, the crystal of growth, 5, silica tube, 6, charge bar, 7, the air outlet, 8, the ellipsoid xenon lamp, 9, melting zone, 10, refrigerating unit, 11, the xenon lamp housing, 12, the crystal growth watch-dog.
Embodiment
The present invention will be further described below in conjunction with embodiment.Used growing apparatus is an optics float-zone crystal growth furnace, model: FZ-T-12000-X-I-S-SU (Crystal Systems Inc.) Japanese Crystal Syst product.Used initial feed is high pure raw material, and purity all is 99.99%, can buy by conventional route.
1. select several values of x, according to molecular formula (Ln
xRe
1-x)
2O
3By the stoichiometric proportion raw materials weighing,, initial feed is Re in crystal growth prescription
2O
3And Ln
2O
3, chemical equation is: xLn
2O
3+ (1-x) Re
2O
3=(Ln
xRe
1-x)
2O
3
2. the raw material with institute's weighing mixes, and puts into the Pt crucible at 1000～1100 ℃ of sintering, and it is synthetic that insulation 8h carries out sintering.
3. will synthesize good polycrystal and wear into fine powder, in the long balloon of packing into,, make two charge bars, put into 1500 ℃ of sintering 5h of whirl-sintering furnace, obtain the polycrystalline charge bar through vacuumizing and the hydrostatic compacting.
4. two synthetic polycrystalline charge bars are packed in the stove of floating region, one of them under the oxygen atmosphere protection, adopts the growth of xenon lamp heating float-zone method as seed crystal, for preventing crystal cleavage, wants slow cooling after the crystal growth is complete, and temperature fall time is 5 hours.
Embodiment 1:Nd:Lu
2O
3Crystal
Preparation (Nd
xLu
1-x)
2O
3, concrete chemical equation is: xNd
2O
3+ (1-x) Lu
2O
3=(Nd
xLu
1-x)
2O
3
The raw material that present embodiment adopts is Nd
2O
3And Lu
2O
3, get x=0.01 in the proportioning, with Nd
2O
3(4N) and Lu
2O
3(5N) raw material; suitable drying in air; then by the strict weighing of stoichiometric proportion; and abundant mixing; put into the Pt crucible 1000～1100 ℃ of sintering 8 hours; the polycrystal material that obtains is worn into fine powder average grain diameter 4 μ m; getting 30g and 15g polycrystal material is respectively charged in two long balloons; use the glass bar compacting; put into after vacuumizing under the hydrostatic pressing 68KN and suppressed 1 minute; make respectively 2 round charge bars; diameter all is 10mm; length is respectively 80mm and 40mm; 1500 ℃ of lower sintering 5h in whirl-sintering furnace then; with the length that obtains; short 2 polycrystalline rods are packed in the stove of floating region; on in optics float zone growth stove; fix respectively two polycrystalline rods on the position of unloading rod bar; long charge bar is fixed on the loading rod bar; short charge bar is fixed on the unloading rod bar, is warming up to 2500 ℃, the upper end fusing of the lower end of top charge bar and below seed crystal rod with 4 hours; contact begins growth; the growth temperature interval is 2400-2500 ℃, and growth rate and brilliant rotational speed rate are respectively 5-8mm/h and 25r/min, and growth atmosphere is the oxygen protection; oxygen purity is 99.9%, and the oxygen ventilation amount is 50mL/min.
Growth for preventing crystal cleavage, uses 5 hours slow coolings to room temperature after finishing at least.The crystal that takes out from stove, color be the white transparent black of deepening gradually to the top to be from the bottom.Then crystal is carried out anneal,, drop to room temperature with 30 ℃ speed per hour then 1200 ℃ of down insulations 30 hours.After anneal, it is transparent that crystal becomes white, and black disappears.Then the crystal of growth is processed, polished.
Embodiment 2:Nd:Sc
2O
3Crystal
Preparation (Nd
xSc
1-x)
2O
3, chemical equation: xNd
2O
3+ (1-x) Sc
2O
3=(Nd
xSc
1-x)
2O
3
The raw material that present embodiment adopts is Nd
2O
3And Sc
2O
3, get x=0.01 in the proportioning, with Nd
2O
3(4N) and Sc
2O
3(5N) high pure raw material, suitable drying in air then by the strict weighing of stoichiometric proportion, and abundant mixing, is put into the Pt crucible 1000～1100 ℃ of sintering sintering 8 hours, and the polycrystal material that obtains is worn into fine powder, average grain diameter 4 μ m.
Method by embodiment 1 makes in 2 polycrystalline charge bars and the float zone growth stove of packing into; be warming up to the lower end of top charge bar and the upper end fusing of seed crystal rod; contact begins growth; the growth temperature interval is 2400-2500 ℃; growth rate and brilliant rotational speed rate are respectively 5-8mm/h and 25r/min, and growth atmosphere is the oxygen protection.Behind the growth ending, for preventing crystal cleavage, be cooled to room temperature in five hours.The crystal that takes out from stove, color be the white transparent black of deepening gradually to the top to be from the bottom.Then crystal is carried out anneal,, drop to room temperature with 30 ℃ speed per hour then 1200 ℃ of down insulations 30 hours.After anneal, it is transparent that crystal becomes white, and black disappears.Then the crystal of growth is processed, polished.
Embodiment 3:Yb:Lu
2O
3Crystal
Preparation (Yb
xLu
1-x)
2O
3, chemical equation: xYb
2O
3+ 1-xLu
2O
3=(Yb
xLu
1-x)
2O
3
The raw material that present embodiment adopts is high-purity Yb
2O
3And Lu
2O
3, get x=0.05 in the proportioning, with Yb
2O
3(4N) and Lu
2O
3(5N) high pure raw material, suitable drying in air then by the strict weighing of stoichiometric proportion, and abundant mixing, is put into the Pt crucible 1000～1100 ℃ of sintering sintering 8 hours, and the polycrystal material that obtains is worn into fine powder.
Method by embodiment 1 makes in the two polycrystalline charge bars and the float zone growth stove of packing into, and all the other growth conditionss are with embodiment 1.Behind the growth ending, be cooled to room temperature through five hours.The crystal that takes out from the stove of floating region is water white transparency.After this Yb:Lu
2O
3The annealing of crystal, processing is with embodiment 1.
Embodiment 4:Yb:Sc
2O
3Crystal
Preparation (Yb
xSc
1-x)
2O
3, chemical equation, xYb
2O
3+ 1-xSc
2O
3=(Yb
xSc
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Yb
2O
3And 5c
2O
3, get x=0.05 in the proportioning.Yb:Sc
2O
3Raw material preparation and crystal growth, annealing, processing are equal to embodiment 1.
Embodiment 5: preparation Yb, Er:Sc
2O
3Crystal
Chemical equation: xyYb
2O
3+ x (1-y) Er
2O
3+ (1-x) Lu
2O
3=((Yb
yEr
1-y)
xLu
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Yb
2O
3, Ho
2O
3And Lu
2O
3, get x=0.05 in the proportioning, y=0.9.Yb, Ho:Lu
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 6: preparation Yb, Er:Lu
2O
3Crystal
Chemical equation: xyYb
2O
3+ (1-y) xEr
2O
3+ (1-x) Lu
2O
3=((Yb
yEr
1-y)
xLu
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Yb
2O
3, Er
2O
3And Lu
2O
3, get x=0.05 in the proportioning, y=0.9, Yb, Er:Lu
2O
3Raw material preparation and crystal growth, annealing, processing are with embodiment 1.
Embodiment 7: preparation (Er
xLu
1-x)
2O
3Crystal
Chemical equation: xEr
2O
3+ (1-x) Lu
2O
3=(Er
xLu
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Er
2O
3And Lu
2O
3, get x=0.03 in the proportioning.Er:Lu
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 8: preparation (Er
xSc
1-x)
2O
3Crystal
Chemical equation: xEr
2O
3+ 1-xSc
2O
3=(Er
xSc
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Er
2O
3And Sc
2O
3, get x=0.03 in the proportioning.Er:Sc
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 9: preparation (Ho
xSc
1-x)
2O
3Crystal
Chemical equation: xHo
2O
3+ 1-xSc
2O
3=(Ho
xSc
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Ho
2O
3And Lu
2O
3, get x=0.005 in the proportioning.Ho:Sc
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 10: preparation (Ho
xLu
1-x)
2O
3Crystal
Chemical equation: xHo
2O
3+ 1-xLu
2O
3=(Ho
xLu
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Ho
2O
3And Lu
2O
3, get x=0.005 in the proportioning.Ho:Lu
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 11: preparation Ho, Tm:Lu
2O
3Crystal
Chemical equation: x (1-y) Ho
2O
3+ xyTm
2O
3+ (1-x) Lu
2O
3=((Ho
1-yTm
y)
xLu
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Ho
2O
3, Tm
2O
3And Lu
2O
3, get x=0.05 in the proportioning, y=0.9.Ho, Tm:Lu
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 12: preparation Ho, Tm:Sc
2O
3Crystal
Chemical equation: x (1-y) Ho
2O
3+ xyTm
2O
3+ 1-xSc
2O
3=((Ho
1-yTm
y)
xSc
1-x)
2O
3, the raw material that present embodiment adopts is high-purity Ho
2O
3, Tm
2O
3And Sc
2O
3, get x=0.05 in the proportioning, y=0.9.Ho, Tm:Sc
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 13:Nd:(Lu
zY
1-z)
2O
3Crystal
Chemical equation: z (1-x) Lu
2O
3+ (1-z) (1-x) Y
2O
3+ xNd
2O
3=(Nd
x(Lu
zY
1-z)
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity N d
2O
3, Y
2O
3And Lu
2O
3, get x=0.01 in the proportioning, z=0.5.Nd:(Lu
zY
1-z)
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 14: preparation Nd:(Sc
zY
1-z)
2O
3Crystal
Chemical equation: z (1-x) Sc
2O
3+ (1-x) (1-z) Y
2O
3+ xNd
2O
3=(Nd
x(Sc
zY
1-z)
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity N d
2O
3, Sc
2O
3And Y
2O
3, get x=0.01 in the proportioning, z=0.5, Nd:(Sc
zY
1-z)
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 15: preparation Yb:(Lu
zY
1-z)
2O
3Crystal
Chemical equation: z (1-x) Lu
2O
3+ (1-x) (1-z) Y
2O
3+ xYb
2O
3=(Yb
x(Lu
zY
1-z)
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Yb
2O
3, Y
2O
3And Lu
2O
3, get x=0.05 in the proportioning, z=0.5.Nd:(Lu
zY
1-z)
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Embodiment 16: preparation Yb:(Sc
zY
1-z)
2O
3Crystal
Chemical equation: z (1-x) Sc
2O
3+ (1-x) (1-z) Y
2O
3+ xYb
2O
3=(Yb
x(Sc
zY
1-z)
1-x)
2O
3,
The raw material that present embodiment adopts is high-purity Yb
2O
3, Y
2O
3And Sc
2O
3, get x=0.05 in the proportioning, z=0.5.Nd:(Sc
zY
1-z)
2O
3Raw material preparation and crystal growth, annealing, processing is with embodiment 1.
Claims (7)
1. rare earth oxide laser crystal, general formula is: (Ln
xRe
1-x)
2O
3, 0＜x＜0.3,
Wherein, Ln=Yb, Nd, Tm, Er, Ho, Yb
yEr
1-yOr Tm
yHo
1-y0＜y＜1; Re=Lu, Sc, Lu
zY
1-zOr Sc
zY
1-z0＜z＜1, crystal are isometric system, and spacer is Ia3, the bixbyite structure.
2. rare earth oxide laser crystal as claimed in claim 1 is characterized in that,
Work as Ln=Nd, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.05;
Work as Ln=Yb, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.3;
Work as Ln=Er, when Re=Lu or Sc, (Ln
xRe
1-x)
2O
3In 0＜x＜0.03.
3. rare earth oxide laser crystal as claimed in claim 1 is characterized in that, is one of following:
A. (Nd
xLu
1-x)
2O
3, x=0.01, unit cell parameters:
Fusing point: 2510 ℃,
B. (Ln
xSc
1-x)
2O
3, x=0.01, unit cell parameters:
Fusing point: 2450 ℃.
4. the preparation method of the described rare earth oxide laser crystal of claim 1 is with Re
2O
3And Ln
2O
3Be raw material, adopt the floating zone method growth, used grower is optics float zone growth stove, adopts four xenon lamp heating, and crystal growth step comprises:
(1) according to (Ln
xRe
1-x)
2O
3The molar ratio weighing raw material of each component and mixing in the formula is put into the Pt crucible at 1000～1100 ℃ of sintering, and insulation 8h gets polycrystal material, and is for subsequent use;
(2) with agate mortar polycrystal is ground, be milled into fine powder, median size 4 μ m get 20-30g and 15-20g material respectively and pack in two balloons; Vacuumize after installing,, make two poles that diameter is identical, length is different 68KN hydrostatic compacting 1-1.5 minute, and then in whirl-sintering furnace 1500 ℃ burnt 4-5 hour, polycrystalline rod;
(3) in optics float zone growth stove, fix long and short two polycrystalline rods on the position of upper and lower charge bar bar respectively, a wherein following polycrystalline rod is the seed crystal rod, above a polycrystalline rod be charge bar, with silica tube seed crystal rod and charge bar are sealed, the program of setting by the float zone growth stove was warming up to 2500 ℃ with 4-4.5 hour, make as the upper end of seed crystal rod and the charge bar lower end fusing of its top and contact, the control growing temperature range is 2400-2500 ℃, set the pull rate and the rotating speed of crystal growth, the beginning crystal growth;
(4) crystal growth finishes, and slowly reduces to room temperature through 5-5.5 hour, and crystal is come out of the stove; The crystal of the coming out of the stove 30-32h that anneals under 1500 ℃ temperature, annealing atmosphere is an atmosphere.
5. preparation method as claimed in claim 4 is characterized in that, the pull rate of crystal growth is 5-8mm/h in the step (3), rotating speed 20-30r/min.
6. preparation method as claimed in claim 4 is characterized in that, the crystal growth in the step (3) is carried out under the oxygen protective atmosphere, and oxygen purity is 99.9%, and the oxygen ventilation amount is 50mL/min.
7. each described rare earth oxide crystal of claim 1～3 is used to make Laser Devices.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949061A (en) * | 2010-10-29 | 2011-01-19 | 中国科学院上海硅酸盐研究所 | Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof |
| CN102534790A (en) * | 2012-01-19 | 2012-07-04 | 山东大学 | Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof |
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| CN104498034A (en) * | 2014-12-17 | 2015-04-08 | 中国科学院上海光学精密机械研究所 | Neodymium ion doped scandium oxide and lutetium oxide mixed crystal laser material and preparation method thereof |
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| CN111041558A (en) * | 2019-07-16 | 2020-04-21 | 中国科学院上海光学精密机械研究所 | Rare earth sesquioxide laser crystal growth method |
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| CN101949061A (en) * | 2010-10-29 | 2011-01-19 | 中国科学院上海硅酸盐研究所 | Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof |
| CN101949061B (en) * | 2010-10-29 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Rare earth-doped lutetium-scandium borate scintillation single crystals and growth method thereof |
| CN102560666B (en) * | 2012-01-19 | 2015-04-22 | 山东大学 | Preparation method of composite laser crystal in garnet structure |
| CN102560666A (en) * | 2012-01-19 | 2012-07-11 | 山东大学 | Preparation method of composite laser crystal in garnet structure |
| CN102560668B (en) * | 2012-01-19 | 2014-09-10 | 山东大学 | Preparation method of vanadate composite laser crystal having zirconite structure |
| CN102534790B (en) * | 2012-01-19 | 2014-11-05 | 山东大学 | Garnet composite crystal with multi-segment doping concentration gradient and growing method thereof |
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| CN104498034B (en) * | 2014-12-17 | 2016-07-06 | 中国科学院上海光学精密机械研究所 | Neodymium ion doped Scia luteium oxide mixed crystal laser material and preparation method thereof |
| CN108221055B (en) * | 2018-01-09 | 2020-10-09 | 上海应用技术大学 | Intrinsically luminous scintillation crystal magnesium tantalate and preparation method and application thereof |
| CN108221055A (en) * | 2018-01-09 | 2018-06-29 | 上海应用技术大学 | A kind of intrinsic luminous scintillation crystal tantalic acid magnesium and its preparation method and application |
| CN108707964A (en) * | 2018-04-13 | 2018-10-26 | 中国电子科技集团公司第十研究所 | Melt crucible and material ingot in the area for being used to prepare molecular beam epitaxy beam source material ingot |
| CN109748585A (en) * | 2019-03-19 | 2019-05-14 | 中国工程物理研究院化工材料研究所 | The efficient preparation Yb:Sc of sintering aid need not be added2O3The method of laser transparent ceramic |
| CN109748585B (en) * | 2019-03-19 | 2021-07-27 | 中国工程物理研究院化工材料研究所 | Sc and Yb are efficiently prepared without adding sintering aids2O3Method for laser-transparent ceramics and ceramics |
| CN111041558A (en) * | 2019-07-16 | 2020-04-21 | 中国科学院上海光学精密机械研究所 | Rare earth sesquioxide laser crystal growth method |
| CN111041558B (en) * | 2019-07-16 | 2021-10-08 | 中国科学院上海光学精密机械研究所 | Rare earth sesquioxide laser crystal growth method |
| WO2022028800A1 (en) * | 2020-08-05 | 2022-02-10 | Forschungsverbund Berlin E.V. | Method and device for growing a rare earth sesquioxide crystal |
| CN113036597A (en) * | 2021-03-05 | 2021-06-25 | 山东大学 | Mode-locked ultrafast intermediate infrared laser and working method and application thereof |
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