CN102674839A - Preparation method of Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material - Google Patents
Preparation method of Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material Download PDFInfo
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Abstract
The invention relates to a preparation method of a Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material, belonging to the field of manufacturing processes of special ceramic materials. The preparation method comprises the following steps: preparing national high-purity (4N purity) Tm2O3 nano powder, La2O3 nano powder and Y2O3 nano powder, which are used as raw materials, in a certain mol ratio, forming by a traditional ceramic preparation technique, and carrying out solid-phase sintering to obtain the compact Tm:Y<2-2x>La<2x>O<3> (namely Y<2-2x-2y>La<2x>Tm<2y>O<3>) transparent ceramic. The Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material has favorable optical properties. The Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material has the advantages of simple preparation technique and low manufacturing cost, and is beneficial to industrial large-scale production. The transmittance light spectrum experiment indicates that the sample has high transmittance near 2 mu m, and has an obvious absorption peak near 800nm, and the LD can be directly used as a pumping source. The fluorescent spectroscopy displays that the peak value is at 1931nm, which indicates that the Tm<3+>-doped yttrium lanthanum oxide laser transparent ceramic material is hopeful to become a 2 mu m laser working medium material.
Description
Technical field
The present invention relates to mix Tm
3+Lanthanum yttrium oxide laser transparent ceramic material and preparation method thereof, it belongs to the special cermacis manufacturing process technology field.
Background technology
2 mu m waveband lasers have obtained application aspect a lot, the characteristics of atmospheric transmission of 2 mu m waveband lasers is good, and is strong to battlefield smog penetrativity, and to eye-safe, lidar militarily also occupies very consequence in addition.2 mu m waveband lasers can also be used as medical surgical knife, do shallow table property operation (can not injure deep layer), guarantee operation safety.
Rare earth ion Tm
3+(thulium) ionic
3F
4→
3H
6Energy level transition is to obtain the luminous main path of 2 mu m wavebands.Tm
3+Ion has little stimulated emission cross section, but because of the cross relaxation process in its energy level excitation process, makes Tm
3+The ion internal quantum efficiency reaches 2, so the Laser emission intensity of its luminous intensity not second to having reported.Research at present is laserable material more widely, mainly is rare earth ion doped crystal and glass material, and YAG (yttrium aluminum garnet) studies morely aspect transparent ceramic material research, and has also realized the output of laser.Because lanthanum yttrium oxide base transparent ceramic material thermal conductivity than the ceramic advantage such as low of YAG, makes the lanthanum yttrium oxide base transparent ceramic material be expected to realize that comparatively ideal laser exports than ceramic high, the phonon energy of YAG.
Y
2O
3Material thermal conductivity is high, is that the twice of YAG is many, and its phonon energy is lower than YAG, is a kind of good Solid State Laser substrate material.But because Y
2O
3Fusing point up to 2430 ℃, and near 2280 ℃ cube polycrystalline phase transformation of six side's phases in opposite directions can take place, thereby be difficult to grow the Y of large size and high optical quality
2O
3Crystal.Along with the development of ceramics processing and nanometer powder-making technique, Y
2O
3The sintering temperature of crystalline ceramics can be reduced to about 1700 ℃.Through at Y
2O
3Add La in the powder
2O
3Powder can promote moving of crystal boundary, quickens pore and gets rid of, and promotes Y
2O
3Ceramic post sintering, so the lanthanum yttrium oxide base transparent ceramic is a kind of laser host material of excellent property.Utilize Tm
3+Ion exists
3F
4→
3H
6Transition on the energy level, thus the laser output of 2 mum wavelengths obtained, mix Tm
3+The lanthanum yttrium oxide laser transparent ceramic is expected to become a kind of 2 μ m laser working medium materials with development potentiality.
Summary of the invention
The objective of the invention is to: adopt homemade high-purity Tm
2O
3, La
2O
3And Y
2O
3Nano powder is a raw material, adopts traditional ceramics preparation technology, adopts suitable sintering method, under lower temperature conditions, adopts solid sintering technology at last, and Tm is mixed in preparation
3+The lanthanum yttrium oxide transparent stupalith.
The present invention relates to mix Tm
3+Lanthanum yttrium oxide laser transparent ceramic preparation methods, its preparation process and step are following:
A. adopt high-purity homemade 99.99% Tm
2O
3, 99.99% La
2O
3And 99.99%Y
2O
3Nano powder is a raw material, and three's mole proportioning is pressed chemical molecular formula Y
2-2x-2yLa
2xTm
2yO
3, the x=0.01 in the formula~0.20, y=0.005 ~ 0.10;
The Y that b. will prepare by said ratio
2-2x-2yLa
2xTm
2yO
3Mixed powder is put into ball grinder and is carried out ball milling, mixed powder ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
C. ball milling is good powder is calcined powder mix in drying in oven then in retort furnace, 1200 ℃ are incubated 10 hours, and naturally cooling obtains Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) powder.
D. once more powder is put into the spheroidal graphite jar and carry out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
E. ball milling is good powder carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
F. the powder after the granulation is dry-pressing formed, depress to the sheet sample in the 200MPa isostatic cool pressing subsequently;
G. said sample is placed in the molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering range is 1600~1700 ℃, and sintering time is 40 ~ 45 hours, the final Tm:Y that obtains densification
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Preceding oneself states, and trial-production can be according to this crystalline ceramics molecular formula: Y
2-2x-2yLa
2xTm
2yO
3, and making x=0.01~0.20, y=0.005 ~ 0.10 can be according to trial-production with x, and the y scope is carried out the combination modulation of series, and for example: fixing x=0.10 can be its y value respectively: y=0.04; Y=0.02; Y=0.06; Y=0.08; Y=0.10; Y=0.01; Y=0.005 or the like
And for example: x=0.08, y=0.02; Y=0.05; As working as: x=0.05, y=0.02; Y=0.04 or the like
Equally: x=0.01, y=0.02; Y=0.05; X=0.20, y=0.02; Y=0.01; Y=0.07 or the like
So own x=0.01~0.20 in this molecular formula of the present invention; Shown in y=0.005 ~ 0.10 and specialized related invention technology, and institute's phasing pass category, and if the simulation of no normal reason; Or analogy; Or extend, promptly shown to relate to institute's phasing pass or similar molecular formula category in the embodied technique of the present invention, also can belong to present technique invention protection authority.
Description of drawings
Fig. 1
,Mix Tm
3+(ordinate is transmitance-% to the optical transmission spectra of lanthanum yttrium oxide laser transparent ceramic, and X-coordinate is a wavelength-nm)
Fig. 2 mixes Tm
3+(ordinate is a fluorescence intensity to the emmission spectrum of lanthanum yttrium oxide laser transparent ceramic, and X-coordinate is a wavelength-nm).
Embodiment
Embodiments of the invention are narrated according to the order of sequence as follows
Embodiment 1
In the present embodiment, Tm is mixed in preparation
3+The concrete process step of lanthanum yttrium oxide laser transparent ceramic is following:
A. adopt high-purity homemade 99.99% Tm
2O
3, 99.99% La
2O
3And 99.99%Y
2O
3Nano powder is a raw material, and three's quality proportioning is pressed chemical molecular formula Y
2-2x-2yLa
2xTm
2yO
3, the x=0.10 in the formula, y=0.04; The molar content of each composition is respectively: Tm
2O
3=0.04mol, La
2O
3=0.10mol, Y
2O
3=0.86mol;
B. by said ratio weighing Tm
2O
3, La
2O
3And Y
2O
3Powder is put into ball grinder and is carried out ball milling, compound ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
C. ball milling is good powder is put into baking oven, and oven dry is calcined powder mix in retort furnace at a certain temperature, 1200 ℃ of insulation 10h, naturally cooling;
D. once more powder is put into ball grinder and carry out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 commentaries on classics/min;
E. ball milling is good powder carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
F. the powder after the granulation is dry-pressing formed, depress to the sheet sample in the 200MPa isostatic cool pressing subsequently;
G. said sample is placed in the molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering temperature is 1680 ℃, and sintering time is 45 hours, the Tm that mixes that finally prepares densification and have favorable optical performance
3+The lanthanum yttrium oxide transparent pottery.
Embodiment 2
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.02; The molar content of each composition is respectively: Tm
2O
3=0.02mol, La
2O
3=0.10mol, Y
2O
3=0.88mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 3
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.06; The molar content of each composition is respectively: Tm
2O
3=0.06mol, La
2O
3=0.10mol, Y
2O
3=0.84mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 4
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.08; The molar content of each composition is respectively: Tm
2O
3=0.08mol, La
2O
3=0.10mol, Y
2O
3=0.82mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 5
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.10; The molar content of each composition is respectively: Tm
2O
3=0.10mol, La
2O
3=0.10mol, Y
2O
3=0.80mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 6
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.01; The molar content of each composition is respectively: Tm
2O
3=0.01mol, La
2O
3=0.10mol, Y
2O
3=0.89mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 7
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.08 in the formula, y=0.02; The molar content of each composition is respectively: Tm
2O
3=0.02mol, La
2O
3=0.08mol, Y
2O
3=0.90mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 8
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.08 in the formula, y=0.05; The molar content of each composition is respectively: Tm
2O
3=0.05mol, La
2O
3=0.08mol, Y
2O
3=0.87mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 9
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.05 in the formula, y=0.02; The molar content of each composition is respectively: Tm
2O
3=0.02mol, La
2O
3=0.05mol, Y
2O
3=0.93mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.05 in the formula, y=0.04; The molar content of each composition is respectively: Tm
2O
3=0.04mol, La
2O
3=0.05mol, Y
2O
3=0.91mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 11
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.01 in the formula, y=0.02; The molar content of each composition is respectively: Tm
2O
3=0.02mol, La
2O
3=0.01mol, Y
2O
3=0.97mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 12
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.05; The molar content of each composition is respectively: Tm
2O
3=0.05mol, La
2O
3=0.10mol, Y
2O
3=0.85mol; 1640 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 13
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.01; The molar content of each composition is respectively: Tm
2O
3=0.01mol, La
2O
3=0.10mol, Y
2O
3=0.89mol; 1640 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 14
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.20 in the formula, y=0.02; The molar content of each composition is respectively: Tm
2O
3=0.02mol, La
2O
3=0.20mol, Y
2O
3=0.78mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 15
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.20 in the formula, y=0.01; The molar content of each composition is respectively: Tm
2O
3=0.01mol, La
2O
3=0.20mol, Y
2O
3=0.79mol; 1640 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 16
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.20 in the formula, y=0.07; The molar content of each composition is respectively: Tm
2O
3=0.07mol, La
2O
3=0.20mol, Y
2O
3=0.73mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 17
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.20 in the formula, y=0.09; The molar content of each composition is respectively: Tm
2O
3=0.09mol, La
2O
3=0.20mol, Y
2O
3=0.71mol; 1680 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 18
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.005; The molar content of each composition is respectively: Tm
2O
3=0.005mol, La
2O
3=0.10mol, Y
2O
3=0.895mol; 1640 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
Embodiment 19
The process step of present embodiment and the foregoing description 1 are identical, and that different is Y
2-2x-2yLa
2xTm
2yO
3X=0.10 in the formula, y=0.01; The molar content of each composition is respectively: Tm
2O
3=0.01mol, La
2O
3=0.10mol, Y
2O
3=0.89mol; 1700 ℃ of sintering temperatures, soaking time 45h obtains fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
By above-mentioned examples preparation fine and close Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics, have the good optical performance.Material preparation process of the present invention is simple, and low cost of manufacture helps industrial scale production.The optical transmission spectra of crystalline ceramics sample adopts the V-570 type UV/VIS/NIR spectrophotometer of Japanese JASCO company to test; As shown in Figure 1; Absorption peak is obvious near can finding its 800nm; Near 2 μ m, higher transmittance is arranged, LD (semiconductor laser) can be directly as pumping source.(Trix-550, Jobin Yvon Spex France) detect emmission spectrum, and be as shown in Figure 2, can find near 2 μ m, to have the emission band of a broad, and the strongest emission peak is positioned at the 1931nm place, and test result is all explained and mixed Tm through fluorescence spectrum analyzer
3+The lanthanum yttrium oxide transparent pottery is expected to become a kind of 2 μ m laser working medium materials.
Claims (2)
1. mix Tm for one kind
3+Lanthanum yttrium oxide laser transparent ceramic preparation methods is characterized in that this laser transparent ceramic has following preparation process:
A. adopt high-purity homemade 99.99% Tm
2O
3, 99.99% La
2O
3And 99.99%Y
2O
3Nano powder is a raw material, and three's mole proportioning is pressed chemical molecular formula Y
2-2x-2yLa
2xTm
2yO
3, the x=0.01 in the formula~0.20, y=0.005 ~ 0.10;
The Y that b. will prepare by said ratio
2-2x-2yLa
2xTm
2yO
3Mixed powder is put into ball grinder and is carried out ball milling, mixed powder ball milling 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 r/min;
C. ball milling is good powder is calcined powder mix in drying in oven then in retort furnace, 1200 ℃ are incubated 10 hours, and naturally cooling obtains Tm:Y
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) powder;
D. once more powder is put into the spheroidal graphite jar and carry out ball milling, ball milling is 5 hours in the alcohol medium, and material ball ratio is 2:1, and the alcohol powder quality is than being 4:1, and drum's speed of rotation is 50 r/min;
E. ball milling is good powder carries out granulation in drying in oven with powder, crosses 40 mesh sieves;
F. the powder after the granulation is dry-pressing formed, depress to the sheet sample in isostatic cool pressing 200MPa condition then;
G. said sample is placed in the silicon molybdenum wire furnace, under the normal pressure reducing atmosphere, carries out sintering; Sintering range is 1700~1800 ℃, and sintering time is 40 ~ 45 hours, the final Tm:Y that obtains densification
2-2xLa
2xO
3(be Y
2-2x-2yLa
2xTm
2yO
3) crystalline ceramics.
2. according to a kind of Tm that mixes of claim 1
3+Lanthanum yttrium oxide laser transparent ceramic preparation methods is characterized in that by chemical molecular formula Y
2-2x-2yLa
2xTm
2yO
3, the x=0.01 in the formula~0.20, y=0.005 ~ 0.10; Can be according to trial-production with x, the y scope is carried out series of combination modulation: fixing x=0.10 can be its y value respectively: y=0.04; Y=0.02; Y=0.06; Y=0.08; Y=0.10; Y=0.01; Y=0.005 or the like; And for example: x=0.08, y=0.02; Y=0.05; As working as: x=0.05, y=0.02; Y=0.04 or the like; Equally: x=0.01, y=0.02; Y=0.05; Or work as x=0.20, y=0.02; Y=0.01; Y=0.07 or the like has shown to relate in the embodied technique of the present invention, and institute's phasing closes or similar molecular formula modulation category ownership eigen.
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CN103601497A (en) * | 2013-10-24 | 2014-02-26 | 上海大学 | Preparation method for Tm<3+> and Yb<3+> co-doped yttrium-lanthanum oxide transparent ceramic material |
CN103964849A (en) * | 2013-10-15 | 2014-08-06 | 上海大学 | Preparation method of Er<3+>, Pr<3+> and Tm<3+>-doped yttrium lanthanum oxidetransparent ceramic for lasers |
CN104150904A (en) * | 2014-05-09 | 2014-11-19 | 上海大学 | Preparation method of Er<3+>-single-doped yttrium lanthanum oxide transparent ceramic for middle infrared lasers |
CN106631022A (en) * | 2017-01-13 | 2017-05-10 | 中国计量大学 | Tm sensitized yttria-based laser ceramic and preparation method |
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CN103073295A (en) * | 2013-01-17 | 2013-05-01 | 上海大学 | Preparation method of Er3+ and Tm3+ co-doped yttrium lanthanum oxide scintillating material transparent ceramic material |
CN103073295B (en) * | 2013-01-17 | 2014-07-30 | 上海大学 | Preparation method of Er3+ and Tm3+ co-doped yttrium lanthanum oxide scintillating material transparent ceramic material |
CN103964849A (en) * | 2013-10-15 | 2014-08-06 | 上海大学 | Preparation method of Er<3+>, Pr<3+> and Tm<3+>-doped yttrium lanthanum oxidetransparent ceramic for lasers |
CN103601497A (en) * | 2013-10-24 | 2014-02-26 | 上海大学 | Preparation method for Tm<3+> and Yb<3+> co-doped yttrium-lanthanum oxide transparent ceramic material |
CN104150904A (en) * | 2014-05-09 | 2014-11-19 | 上海大学 | Preparation method of Er<3+>-single-doped yttrium lanthanum oxide transparent ceramic for middle infrared lasers |
CN106631022A (en) * | 2017-01-13 | 2017-05-10 | 中国计量大学 | Tm sensitized yttria-based laser ceramic and preparation method |
CN106631022B (en) * | 2017-01-13 | 2020-03-24 | 中国计量大学 | Tm sensitized yttrium oxide based laser ceramic and preparation method thereof |
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