CN102674837A - Er<3+>:Lu2O3 transparent ceramic - Google Patents

Er<3+>:Lu2O3 transparent ceramic Download PDF

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CN102674837A
CN102674837A CN2012101603204A CN201210160320A CN102674837A CN 102674837 A CN102674837 A CN 102674837A CN 2012101603204 A CN2012101603204 A CN 2012101603204A CN 201210160320 A CN201210160320 A CN 201210160320A CN 102674837 A CN102674837 A CN 102674837A
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lu2o3
transparent ceramic
crystalline ceramics
emission
ceramics
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王能利
张希艳
王鹏贺
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Changchun University of Science and Technology
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Changchun University of Science and Technology
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Abstract

The invention relates to an Er<3+>:Lu2O3 transparent ceramic, belonging to the technical field of optical functional materials. Er<3+> is doped into an Lu2O3-base transparent ceramic to obtain the Er<3+>:Lu2O3 transparent ceramic. The prior art, a Lu2O3-base transparent ceramic material, which can be excited by 980nm light emitted by an accessible and simple semiconductor laser device, and can acquire 570nm green light emission through upconversion and acquire 1.54 mu m emission through downconversion, is absent. The Er<3+>:Lu2O3 transparent ceramic has an isometric system bixbyite crystal structure, and belongs to an Ia3 space group; and the lattice constant is disclosed in the specification. The invention is characterized in that the chemical molecular formula is (Lu[1-x]Er[x])[2]O[3], wherein x is the mol component of the doping ion Er<3+>, and 0.01<=x<=0.1. The Er<3+>:Lu2O3 transparent ceramic can become a high-quality material for photoconducting devices, laser devices and infrared detectors, and is very suitable to be used in a cosmetic surgery device; and meanwhile, the invention can be used in the fields of full-curing short-wavelength laser devices, three-dimensional stereo display, biomolecular fluorescent marking, infrared radiation detection, biology, environmental detection, military affairs and the like.

Description

Er 3+: Lu 2O 3Crystalline ceramics
Technical field
The present invention relates to a kind of Er 3+: Lu 2O 3Crystalline ceramics is at Lu 2O 3Mix Er in the base transparent ceramic 3+, obtain Er 3+Doping Lu 2O 3Crystalline ceramics belongs to the optical functional materials technical field.
Background technology
The rare earth doping transparent pottery can be compared with conventional laser dielectric material such as monocrystal material as gain medium, and the rare earth doping transparent pottery has the high-dopant concentration characteristics.In addition,, can obtain the large size material, and realize high power laser light output, like the sesquioxide system material according to existing preparation method.
Aspect heat conductivility, Lu 2O 3The thermal conductivity of body material is 12.5w/mk, and current widely used YAG base laserable material thermal conductivity has only 11w/mk, therefore, and Lu 2O 3Body material has very strong thermal shock resistance.See Lu from crystalline structure 2O 3Have cubic crystal structure, the grain growing isotropy is convenient to the design of optical ceramics material.Lu 2O 3Material has very wide valence band and the band gap of conduction band (about 6.5eV), for different types of active ions provide abundant emission level, is a kind of good luminous host material.Simultaneously, Lu 2O 3Laser ceramics and the present application of base YAG laser ceramics more widely compared; Have lower thermal expansivity and effective phonon energy; And higher light conversion efficiency, shorter scintillation response time and the density of Geng Gao; Enable to bear stronger high-energy radiation, suitable environmental field is wider, and this makes Lu 2O 3The crystalline ceramics of base becomes the gain medium material of a kind of ideal high-efficiency ceramic scintillator and superpower laser and short-pulse laser.
Publication number is that the one Chinese patent application of CN101333110A discloses a kind of Nd 3+Doping Lu 2O 3Base transparent ceramic, i.e. Nd 3+: Lu 2O 3Crystalline ceramics, this crystalline ceramics can emission wavelength be the light of 1.079 μ m under the exciting of 808nm wavelength exciting light." Chinese rare-earth journal " the 25th volume the 5th periodical has been stepped on one piece and has been entitled as " Lu 2O 3: Bi 3+The powder crystal Luminescence Study of Modified Porous " article, disclosed technical scheme is Bi 3+: Lu 2O 3Ceramic powder, the emission wavelength under 320 ~ 375nm ultraviolet excitation are the blue light of 490nm.Also has a kind of Eu in the prior art 3+: Lu 2O 3Crystalline ceramics, its excitation spectrum are the 394nm UV-lights, and emission wavelength is the ruddiness of 610nm.
Yet, need a kind of rare earth ion doped Lu in this technical field 2O 3Base transparent ceramic material, this material can be obtained the 570nm green emission and pass through conversion acquisition 1.54 μ m emission down through last conversion, thereby satisfied some practical demand by the 980nm optical excitation that is easy to get and uses simple semiconductor laser to launch.
Summary of the invention
In order to obtain a kind of Lu 2O 3Base transparent ceramic material, this material can be by the optical excitation of 980nm, emission 570nm green glow and 1.54 μ m infrared lights, we have invented a kind of Er 3+: Lu 2O 3Crystalline ceramics.
The present invention's Er 3+: Lu 2O 3Crystalline ceramics has isometric system bixbyite crystalline structure, belongs to the Ia3 spacer, lattice parameter
Figure BDA00001667613100011
It is characterized in that chemical molecular formula is: (Lu 1-xEr x) 2O 3, x is dopant ion Er 3+The mole component, and 0.01≤x≤0.1.
Its effect of the present invention is Er 3+: Lu 2O 3Crystalline ceramics is owing to have single isometric system Lu 2O 3Phase, and do not have other dephasigns, see shown in Figure 1, so optical isotropy, its specific refractory power does not have directivity, makes Lu 2O 3The transparent possibility that becomes of pottery; Have bixbyite crystalline structure, Ia3 spacer, lattice parameter
Figure BDA00001667613100021
Etc. constructional feature, and ceramic crystalline grain size is evenly, size of microcrystal about 12 μ m, ceramic dense structure, intracrystalline and intergranular pore-free and dephasign produce, see shown in Figure 2, through test the present invention's Er 3+: Lu 2O 3Crystalline ceramics has the transmitance greater than 65% at visible light wave range and infrared each wave band, sees shown in Figure 3.With Er 3+: Lu 2O 3The crystalline ceramics sample is processed as the thick thin slice of 1.5mm 1, after surface finish processing, has transparent intuitively form, sees shown in Figure 4.Because Er 3+: Lu 2O 3Crystalline ceramics is changed green emission on excellent having under the 980nm laser excitation, sees shown in Figure 5ly, and this makes it become a kind of fine photoelectric device, laser apparatus, infrared detector material.Because Er 3+: Lu 2O 3Crystalline ceramics has excellent following conversion 1.54 μ m infrared lights emission under 980nm laser excitation, see shown in Figure 6ly, and tissue is strong especially to the photoabsorption of 1.54 μ m, thereby, Er 3+: Lu 2O 3Crystalline ceramics is suitable for use in the plastic surgery operations device very much.Equally, Er 3+: Lu 2O 3Crystalline ceramics can also be applied to solidify full fields such as short wavelength laser, 3 D stereo demonstration, biomolecules fluorescence labelling, infrared detective, biology, environment measuring and military affairs.
Description of drawings
Fig. 1 is the present invention's Er 3+: Lu 2O 3The XRD spectra of crystalline ceramics.Fig. 2 is the present invention's Er 3+: Lu 2O 3The SEM pattern photo of crystalline ceramics sample glazed surface.Fig. 3 is the present invention's Er 3+: Lu 2O 3Crystalline ceramics transmittance curve figure.Fig. 4 is the present invention's Er 3+: Lu 2O 3The sample intuitively transparent form schematic picture of crystalline ceramics after polishing processing.Fig. 5 is the present invention's Er 3+: Lu 2O 3The up-conversion luminescence spectrogram of crystalline ceramics under 980nm laser excitation, this figure is simultaneously as Figure of abstract.Fig. 6 is the present invention's Er 3+: Lu 2O 3The down-conversion luminescence spectrogram of crystalline ceramics under 980nm laser excitation.
Embodiment
Er through the present invention below 3+: Lu 2O 3The preparation of crystalline ceramics further specifies the present invention.
Dopant ion Er 3+The value of mole component x be one of following: 0.01,0.02,0.03,0.1, corresponding Er 3+: Lu 2O 3Er in the crystalline ceramics product 3+Doping content is for being followed successively by 1.0at.%, 2.0at.%, 3.0at.%, 10at.%.Existing with Er 3+Doping content is the Er of 2.0at.% 3+: Lu 2O 3Crystalline ceramics is an example, and the present invention's Er is described 3+: Lu 2O 3The preparation of crystalline ceramics, and then explanation the present invention's Er 3+: Lu 2O 3Crystalline ceramics.Adopt high-purity Lu of commercial 99.99% 2O 3And Er 2O 3, press chemical molecular formula (Lu 0.98Er 0.02) 2O 3The stoichiometric ratio weigh batching of confirming gets compound, adds tetraethoxy and the mixing of the 0.5wt.% of this compound weight, adds ethanol and thorough mixing again.To be mixed with tetraethoxy, alcoholic acid Lu 2O 3And Er 2O 3Compound places dry grinding granulation in the high speed ball mill, and zirconium ball ball milling 24 hours goes out the powder compound.This powder compound was dried 24 hours under 100 ℃ of temperature; Put into corundum crucible afterwards and place resistance furnace, calcined 3 hours down, put into high speed ball mill afterwards again at 1000 ℃; The granulation of dry grinding once more; Put into the pressure compression molding of punching block after the oven dry earlier, through the 200MPa cold isostatic compaction, obtain biscuit of ceramics again with 30MPa.This biscuit of ceramics is placed the vacuum oven densification sintering, and concrete technology is incubated 1 hour for the temperature rise rate with 5 ℃/min rises to 1400 ℃; Temperature rise rate with 2 ℃/min rises to 1700 ℃ again, is incubated 10 hours, obtains the 2.0at.%Er of highly transparent 3+: Lu 2O 3Crystalline ceramics.

Claims (2)

1. Er 3+: Lu 2O 3Crystalline ceramics has isometric system bixbyite crystalline structure, belongs to the Ia3 spacer, lattice parameter
Figure FDA00001667613000011
It is characterized in that chemical molecular formula is: (Lu 1-xEr x) 2O 3, x is dopant ion Er 3+The mole component, and 0.01≤x≤0.1.
2. Er according to claim 1 3+: Lu 2O 3Crystalline ceramics is characterized in that, dopant ion Er 3+The value of mole component x be one of following: 0.01,0.02,0.03,0.1, corresponding Er 3+: Lu 2O 3Er in the crystalline ceramics product 3+Doping content is for being followed successively by 1.0at.%, 2.0at.%, 3.0at.%, 10at.%.
CN2012101603204A 2012-05-22 2012-05-22 Er<3+>:Lu2O3 transparent ceramic Pending CN102674837A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236980A (en) * 2015-11-19 2016-01-13 中国工程物理研究院化工材料研究所 ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic
CN106588014A (en) * 2016-12-19 2017-04-26 中国科学院长春光学精密机械与物理研究所 Luminescence enhanced Tm<3+>-doped Lu2O3-based transparent ceramic and preparation method thereof
CN107056297A (en) * 2017-03-03 2017-08-18 中国科学院长春光学精密机械与物理研究所 Re:Lu2O3Crystalline ceramics and its gel injection moulding preparation
CN115215651A (en) * 2022-01-09 2022-10-21 上海御光新材料科技股份有限公司 Preparation method of rare earth doped lutetium oxide based composite luminescent ceramic

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CN1587187A (en) * 2004-08-04 2005-03-02 中国科学院上海硅酸盐研究所 Lanthanum hafnate base transparent ceramics and its preparing method
CN101333110A (en) * 2008-07-16 2008-12-31 上海大学 Method for preparing Nd<3+> -doped Lu2O3transparent laser ceramic

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105236980A (en) * 2015-11-19 2016-01-13 中国工程物理研究院化工材料研究所 ZrO2-LiF-codoped vacuum sintering method for lutetium oxide transparent ceramic
CN106588014A (en) * 2016-12-19 2017-04-26 中国科学院长春光学精密机械与物理研究所 Luminescence enhanced Tm<3+>-doped Lu2O3-based transparent ceramic and preparation method thereof
CN106588014B (en) * 2016-12-19 2019-08-23 中国科学院长春光学精密机械与物理研究所 A kind of Tm of luminescence enhancement3+Adulterate lutecia based transparent ceramics and preparation method
CN107056297A (en) * 2017-03-03 2017-08-18 中国科学院长春光学精密机械与物理研究所 Re:Lu2O3Crystalline ceramics and its gel injection moulding preparation
CN115215651A (en) * 2022-01-09 2022-10-21 上海御光新材料科技股份有限公司 Preparation method of rare earth doped lutetium oxide based composite luminescent ceramic

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Application publication date: 20120919