CN106835261B - A kind of growing method and application thereof - Google Patents

A kind of growing method and application thereof Download PDF

Info

Publication number
CN106835261B
CN106835261B CN201710057088.4A CN201710057088A CN106835261B CN 106835261 B CN106835261 B CN 106835261B CN 201710057088 A CN201710057088 A CN 201710057088A CN 106835261 B CN106835261 B CN 106835261B
Authority
CN
China
Prior art keywords
laser
crystal
tabletting
nano
crystallite
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710057088.4A
Other languages
Chinese (zh)
Other versions
CN106835261A (en
Inventor
曾和平
江梦慈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Huapu Quantum Technology Co ltd
Original Assignee
East China Normal University
Shanghai Langyan Optoelectronics Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by East China Normal University, Shanghai Langyan Optoelectronics Technology Co Ltd filed Critical East China Normal University
Priority to CN201710057088.4A priority Critical patent/CN106835261B/en
Publication of CN106835261A publication Critical patent/CN106835261A/en
Application granted granted Critical
Publication of CN106835261B publication Critical patent/CN106835261B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B1/00Single-crystal growth directly from the solid state
    • C30B1/02Single-crystal growth directly from the solid state by thermal treatment, e.g. strain annealing
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B30/00Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/02Heat treatment

Abstract

The present invention provides a kind of growing methods and application thereof comprising following steps: S1: after mixing by crystal growth material and compound containing ytterbium ion, being pressed into tabletting;S2: the tabletting is subjected to laser sintered growth, obtains crystallite or nano-crystal;S3: adjustment laser spot size makes the laser facula cover entire seed crystal surface, carries out in-situ annealing, obtain crystal.The growing method can be used for the preparation of ceramics.It is a kind of high-efficient the present invention is based on studying, stability is good, the low growing method of equipment cost, using the laser sintered method of substep, laser power density needed for the laser sintered process of second step will be well below laser power density needed for process laser sintered in the first step, laser power can be substantially reduced in this way, so that crystal growth equipment becomes to be very easy to satisfaction, and reduce energy consumption.

Description

A kind of growing method and application thereof
Technical field
The present invention relates to crystal preparation fields, more specifically to a kind of High-quality crystal growth method and application thereof.
Background technique
Substance, by gas phase, liquid phase, solid phase transformation, is formed specific under the conditions ofs certain temperature, pressure, concentration, medium, pH etc. The process of dimension sized crystals is known as crystal growth.
Growing method mainly has terraced method of czochralski method, heat-exchanging method, EFG technique, Bridgman-Stockbarger method, kyropoulos, temperature etc.. High temperature refractory oxide is generallyd use in czochralski method, such as zirconium oxide, aluminium oxide make thermal insulation material, make in furnace body in weak oxide gas Atmosphere has oxidation to crucible, and is easy to cause dirt miscellaneous melt, in crystal the defects of formation wrappage, and for those Reactivity is compared with strong or high fusing point material, it is difficult to find suitable crucible to contain them.Heat-exchanging method is in growth crystal mistake It needs ceaselessly to pass to flowing helium in journey and carries out heat exchange, so the consumption of helium is quite big, growth crystal cost is very high. The crystal that volume increases when Bridgman-Stockbarger method is unsuitable for being grown in crystallization, the crystal of growth usually have biggish internal stress, simultaneously It is also difficult to directly observe in crystal growing process, growth cycle is long.Kyropoulos pass through top seed crystal seeding after, not to Upper to lift but steep long crystalline substance, the crystal of growth in the melt and do not contact with crucible, dislocation density is low, monocrystalline good, but crystal is raw The long accumulation for relying on artificial experience strongly, the consistency and yield rate of crystal are poor.The warm ladder entire grower of method is in opposite Stable state, crucible and seed crystal do not rotate, and not only not because of free convection caused by fusant density in such crucible, but also do not have Because of forced convection caused by mechanical stirring, solid liquid interface is interference-free, has more stable thermal field.
Summary of the invention
In view of this, the present invention provides, one kind is high-efficient, and stability is good, the low growing method of equipment cost and its use On the way.
The present invention is achieved by the following technical solutions:
The present invention provides a kind of growing methods comprising following steps:
S1: after mixing by crystal growth material and compound containing ytterbium ion, it is pressed into tabletting;
S2: the tabletting is subjected to laser sintered growth, obtains crystallite or nano-crystal;
S3: adjustment laser spot size makes the laser facula cover entire seed crystal surface, carries out in-situ annealing, Obtain crystal.
The laser is issued by continuous high power laser, and the superpower laser Output of laser wavelength is in quick In the RESONANCE ABSORPTION band for changing ion, with sensitized ions ytterbium ion (Yb3+) for, can be wavelength is 915nm/940nm/960nm/ High-power semiconductor laser etc. near 976nm realizes ytterbium ion (Yb3+) resonance intensify.
Environment of crystal growth can be in air, or vacuumizes or is placed in protective atmosphere again after vacuumizing;It is described Vacuumize the vacuum degree for referring to that extraction meets crystal growth requirement;According to the requirement of growth crystal property, may continue to entire Crystal growing process until entire crystal growth process terminates, or continues to that the laser sintered process of the first step terminates;The pumping Being placed in protective atmosphere after vacuum again is to be placed in protection gas again after vacuumizing process according to the requirement of growth crystal property Atmosphere, the protective gas can be inert atmosphere, can be reducing atmosphere, can be mobility, is also possible to illiquidity , it relative to atmospheric pressure, can be normal pressure, be also possible to negative pressure.
Preferably, step S2 specifically includes following operation:
The tabletting is placed in refractory ceramics container, and output laser facula is focused on wafer surface, so After adjust laser output power so that tabletting is warming up to molten condition at laser focusing;
Laser power is slowly reduced, in-situ annealing is carried out;
When tabletting is cooled to room temperature, former melt region grows crystallite or nano-crystal.
Preferably, step S3 specifically includes following operation:
Adjust laser output power, namely change laser power density so that the crystallite or nano-crystal be warming up to again it is molten Melt state;
Control output laser power, so that melt region is to outer ring from slowly spreading at crystallite or nano-crystal, until set Fusion range;
Laser power is slowly reduced again, and in-situ annealing avoids the thermal stress generated because cooling velocity is too fast;
When tabletting is cooled to room temperature, former melt region grows required crystal.
Preferably, in step S3 required laser power density will it is laser sintered well below in step S2 during Required laser power density.
Preferably, in step S2 and step S3, the temperature of laser sintered active region is real-time by infrared radiation thermometer Monitoring intensifies the upconversion emission intensity distribution real-time monitoring under the laser action of sintering in resonance by sensitized ions.
Preferably, the sensitized ions are ytterbium ion.Ytterbium oxide can be derived from, ytterbium, the packet such as ytterbium chloride are fluorinated Compound containing ytterbium ion;Yb3+With wider absorption band, allow to realize absorption band using the pump light source of wider wave-length coverage Resonance intensify, this is highly advantageous to semiconductor laser is used;Two or more Yb3+Absorb pump light from ground state transition to swash State is sent out, energy transfer when being returned to ground state makes active ions from the upward transition of ground state to active ions;Catalyzing activation ion Pyroreaction;Resonance intensifies sensitized ions such as ytterbium ion (Yb3+) intensify it to height to intensify state, RESONANCE ABSORPTION enhances to photon The absorption of energy, by energy transfer to active ions, radiationless transition improve mixing and doping local temperature and activate from The activity of the solid phase reaction of son.
The present invention also provides a kind of purposes of growing method as the aforementioned in ceramic system is standby.
Basic principle of the invention is:
The growing method includes that laser resonant intensifies the chemical reaction of sensitized ions catalysis high temperature solid-state, laser substep is burnt Knot induction crystallite or nano-crystal catalysis high temperature solid state reaction, laser resonant intensify crystallite or nano-crystal self-diffusion catalysis high temperature solid state reaction Equal core processes;On the one hand, while laser sintered, resonance intensifies rare earth sensitized ions and realizes energy transfer with active ions Intensify again, state is intensified based on rare earth ion and is catalyzed laser sintered high temperature solid state reaction, on the other hand, passes through distribution sintering growth Sensitization containing rare earth/active ions crystallite or nano-crystal, Induced hyperthermia solid phase reaction self-diffusion catalysis reduce laser on the whole and burn Temperature and energy consumption needed for tying high temperature solid state reaction, promote the controllability of sintering process, realize laser sintered large area from expansion Dissipate crystal growth.
It is that the catalysis of the state of intensifying based on sensitized ions is high that laser resonant, which intensifies sensitized ions catalysis high temperature solid-state chemical reaction, Warm solid state reaction process.By rare earth ion mixing and doping sensitization with (or) active ions, induce the laser of sensitized ions Resonance intensify, sensitized ions intensify state to the energy transfer of active ions, active ions intensify state intensify again and multistep cascade Intensify and the cooperation of sensitized ions intensifies and energy transfer etc., in the adjoint radiationless transition humidification area of energy transfer Temperature, intensifying to the high rare earth sensitized ions for intensifying state and rare earth activation ion has better high-temperature catalytic activity, to urge Change laser sintered high temperature solid state reaction, goes out crystallite or nano-crystal in laser sintered region growing.
Laser step sintering induction crystallite or nano-crystal catalysis high temperature solid state reaction process include: first in film micro area laser resonant Intensify sintering, micro-crystal or nanocrystal are grown after annealing;Then laser sintered again in big regional scope, it realizes micro- The resonance of brilliant or nano-crystal intensifies and is catalyzed enhancing.The crystallite or nano-crystal of previous one-step growth in laser sintered step by step, in subsequent point In cloth sintering, on the one hand enhance sensitized ions to the RESONANCE ABSORPTION of laser, on the other hand it is relevant to intensify state energy transfer for enhancing Catalytic action, it can be ensured that be catalyzed high temperature solid state reaction under lower laser power density.
Laser resonant intensifies crystallite or nano-crystal self-diffusion catalysis high temperature solid state reaction process is as follows: dropping in big regional scope Low laser power density implements sintering, and one makes first only in crystallite or nano-crystal periphery catalysis high temperature solid state reaction, then from Crystallite or the diffusion of nano-crystal periphery finally realize that crystallite or nano-crystal are catalyzed oneself of high temperature solid state reaction in entire laser-irradiated domain Diffusion;Furthermore the crystallite or nano-crystal in laser sintered region provide seed crystal grain, conducive to the growth of high-quality crystal.
Compared with prior art, the present invention have it is following the utility model has the advantages that
A kind of high-efficient the present invention is based on studying, stability is good, the low growing method of equipment cost, uses substep Laser sintered method, laser power density needed for the laser sintered process of second step will be well below mistake laser sintered in the first step Laser power density needed for journey can substantially reduce laser power in this way, so that crystal growth equipment becomes to be very easy to completely Foot, and reduce energy consumption;Not all raw material melts simultaneously in raw material melting process, requires the crucible of carrying raw material not tight It is severe, extremely high-temperature crucible container is not needed, and extend the use time of the containers such as crucible;High power continuous laser fuel factor Relatively strong, the heating of crystal growth raw material is very fast, so that rate of crystalline growth is quickly, it is high that the method grows crystal efficiency.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention, Objects and advantages will become more apparent upon:
Fig. 1 is a kind of crystal growing apparatus structural schematic diagram of the present invention;
Fig. 2 is a kind of ceramic grower structural schematic diagram of the present invention.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection scope.
The structure of crystal growing apparatus provided by the invention is as shown in Figure 1, comprising: laser 101, focusing component, reaction Room 502, infrared radiation thermometer 401, annular powder feeder 301, laser sintered effect platform 302 and moveable piston 501, move and live Plug 501 is movably set in reaction chamber 502, and laser sintered effect platform 302 is set to 501 surface of moveable piston, and annular is sent Powder device 301 is set to the surface of laser sintered effect platform 302, and focusing component is set to the oral area of annular powder feeder 301, swashs Light device 101 is set to the side of focusing component, and focusing component includes: collimation lens 201, reflecting mirror 202 and condenser lens 203, Laser from laser injection after, by collimation lens 201 be straightened after, inject reflecting mirror 202, by reflecting mirror 202 reflection, Condenser lens 203 is injected, laser sintered effect platform 302 is transmitted through by condenser lens 203;Infrared radiation thermometer 401 and laser are burnt Knot effect platform 302 is in contact.
The structure of ceramics grower provided by the invention is as shown in Fig. 2, include
Embodiment 1
The present embodiment is related to a kind of growing method, includes the following steps:
By calcirm-fluoride (GaF2) powder and ytterbium oxide (Yb2O3) powder according to molar ratio 1:0.075 ratio weigh 30g, The quality of middle calcirm-fluoride powder is 21.8g, and the quality of ytterbium oxide powder is 8.2g.Powder is put into mortar, is sufficiently stirred It is even, powder is fused together as far as possible.Mixed-powder is placed in annular powder feeder 301, powder passes through annular powder feeding Device nozzle, uniformly output is on laser sintered effect platform 302.Annular powder feeder is controlled by external program, thus it is possible to vary is sent Powder time and powder feeding rate.
Package unit is placed in after vacuumizing in the closed environment 502 for being filled with argon gas (Ar) atmosphere.What this experiment used swashs Light device 101 is semiconductor laser, and Output of laser wavelength 976nm, laser is by coupling fiber-optic output output.Laser first passes through One piece of collimation lens 201 is crossed, the diverging hot spot of output is collimated, then by one piece of reflecting mirror 202, changes laser transmission direction, Again by one piece of condenser lens 203, by hot spot focus processing.In experimentation, pass through 401 real-time monitoring laser of infrared radiation thermometer The temperature in agglomeration area.When monitoring temperature reaches fusing point, it can determine that raw material starts to melt.Laser sintered platform 302 It is placed in moveable piston 501, the movement of piston is controlled by computer program.When laser output laser power is constant, lead to Cross the position for changing piston, it can change the area of output laser facula (acting on laser sintered platform), namely change The power density of laser.Firstly, adjusting at laser sintered platform 302 to laser focusing focus, laser power density reaches at this time Maximum value.Laser output power is adjusted, when laser output laser power reaches 1.17W/mm2When, powder at laser focusing Start to melt, forms melting charge.It is for 10 seconds, then reduce laser output power.It is 500mW/1min that power, which reduces speed, Avoid the thermal stress generated because cooling velocity is too fast.After 7 minutes, the cooling annealing of former melt region is completed, and grows seed crystalline substance Body.
501 position of piston, namely laser sintered 302 position of platform of adjustment are adjusted, so that laser facula becomes larger, covering Powder surface.Equally, pass through the temperature of the laser sintered active region of 401 real-time monitoring of infrared radiation thermometer.Adjust laser output work Rate, when laser output laser power density reaches 0.026W/mm2When, powder surface seed crystal nearby is first begin to reach Fusing point, into melting state.Over time, melt region can from seed crystal region slowly to outer ring spread, when When duration reaches 13 minutes, powder surface is all melted, and is melted with a thickness of 1mm.Then laser output power is reduced.This When melt region area it is larger, power reduce speed be adjusted to 200mW/1min, avoid the heat generated because cooling velocity is too fast Stress.After 15 minutes, the cooling annealing of melt region is completed, and crystal growth is completed.
The structure of ceramics preparation facilities provided by the invention is as shown in Fig. 2, include reaction chamber 502, laser 101, reflection Mirror 202, condenser lens 203, powder delivery conduit 5, mobile work platform 10 and ball mill 9, condenser lens are set to reaction The surface of room 502, reflecting mirror 202 are set to the top of condenser lens 203, and laser 101 is set to the one of mirror lens 202 Side, powder delivery conduit 5 are arranged in reaction chamber 502, and mobile work platform 10 is movably set in the bottom of reaction chamber 502, The top of reaction chamber 502 is additionally provided with air inlet 5021, and ball mill 9 is set on mobile work platform 10.
Embodiment 2
A kind of preparation method for ceramics that the present embodiment is related to, includes the following steps:
By aluminium oxide (Al2O3) powder and ytterbium oxide (Yb2O3) powder according to molar ratio 1:1 ratio weigh 50g, sufficiently Grinding stirs evenly.Mixed-powder is by powder delivery conduit 5, and uniformly output passes through ball milling on mobile work platform 10 Powder surface is flattened and is compacted by machine 9, forms regular tabletting shape 8.
Argon gas (Ar) is filled with into the reaction chamber 502 by air inlet 5021, so that ceramic growth course is in indifferent gas In body atmosphere.Laser 1 is semiconductor laser, and Output of laser wavelength 976nm, it is defeated that laser passes through coupling fiber-optic output Out.Laser changes laser transmission direction by one piece of reflecting mirror 202, then by one piece of condenser lens 203, at hot spot focusing Reason.The temperature of 401 real-time monitoring ceramics vitellarium of infrared radiation thermometer.Mobile work platform 10 is adjusted, i.e. change workbench Upper laser facula area, so that spot diameter reaches 10mm, when adjusting laser output power to 180W, hot spot is covered at powder Start to melt, into liquid phase ceramics synthetic state.After 4 minutes, laser output power is slowly reduced.
Laser output power is adjusted again to 150W, and the duration is still 4 minutes, slowly reduces laser output again Power;It repeats the above steps 10 times, obtained sintered product is aluminium oxide ceramics.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring substantive content of the invention.

Claims (4)

1. a kind of growing method, which comprises the steps of:
S1: after mixing by crystal growth material and compound containing ytterbium ion, it is pressed into tabletting;
S2: the tabletting is subjected to laser sintered growth, obtains crystallite or nano-crystal;
S3: adjustment laser spot size makes the laser facula cover entire seed crystal surface, carries out in-situ annealing, obtain Crystal;
Step S2 specifically includes following operation:
The tabletting is placed in refractory ceramics container, and output laser facula is focused on wafer surface, is then adjusted Whole laser output power, so that tabletting is warming up to molten condition at laser focusing;
Laser power is reduced, in-situ annealing is carried out;
When tabletting is cooled to room temperature, former melt region grows crystallite or nano-crystal;
Step S3 specifically includes following operation:
Laser output power is adjusted, namely changes laser power density, so that the crystallite or nano-crystal are warming up to molten again State;
Control output laser power, so that melt region is to outer ring from spreading at crystallite or nano-crystal, until set melting model It encloses;
Laser power is reduced again, and in-situ annealing avoids the thermal stress generated because cooling velocity is too fast;
When tabletting is cooled to room temperature, former melt region grows required crystal.
2. growing method as described in claim 1, which is characterized in that in step S2 and step S3, laser sintered effect The temperature in area by infrared radiation thermometer real-time monitoring or by sensitized ions resonance intensify under the laser action of sintering upper turn Change spectral intensity distribution real-time monitoring.
3. growing method as claimed in claim 2, which is characterized in that the sensitized ions are ytterbium ion.
4. a kind of purposes of growing method as described in claim 1 in ceramic system is standby.
CN201710057088.4A 2017-01-23 2017-01-23 A kind of growing method and application thereof Active CN106835261B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710057088.4A CN106835261B (en) 2017-01-23 2017-01-23 A kind of growing method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710057088.4A CN106835261B (en) 2017-01-23 2017-01-23 A kind of growing method and application thereof

Publications (2)

Publication Number Publication Date
CN106835261A CN106835261A (en) 2017-06-13
CN106835261B true CN106835261B (en) 2019-03-15

Family

ID=59122453

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710057088.4A Active CN106835261B (en) 2017-01-23 2017-01-23 A kind of growing method and application thereof

Country Status (1)

Country Link
CN (1) CN106835261B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112897528B (en) * 2021-03-24 2022-11-22 云南华谱量子材料有限公司 Method for synthesizing boron carbide/carbon powder material by laser sintering

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1351641A (en) * 1999-03-19 2002-05-29 拉特格斯州立大学 Rare earth doped host materials
CN1428395A (en) * 2001-12-24 2003-07-09 长春科润光电子材料科技有限公司 Red colour conversion material
CN101618946A (en) * 2009-07-03 2010-01-06 中南大学 Yb<3+>-doped oxyfluoride transparent microcrystal glass material and preparation method thereof
CN103666475A (en) * 2013-12-11 2014-03-26 昆明理工大学 Rare earth doped glass frequency conversion luminous material and preparation method thereof
CN103803804A (en) * 2012-11-14 2014-05-21 中国科学院上海硅酸盐研究所 Nano glass ceramic up-conversion luminescent material and preparation method thereof
CN105602566A (en) * 2016-02-29 2016-05-25 武汉理工大学 Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof
CN106010536A (en) * 2016-05-26 2016-10-12 中国科学院宁波材料技术与工程研究所 Method for synthesizing monodisperse rare earth doped up-converted fluorescence nanocrystalline through microwave assistance, and product thereof and application
CN106082676A (en) * 2016-06-06 2016-11-09 中国科学院上海光学精密机械研究所 Mix the INFRARED ABSORPTION height Aluminous Silicate Glass-Ceramics of samarium, ytterbium

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1351641A (en) * 1999-03-19 2002-05-29 拉特格斯州立大学 Rare earth doped host materials
CN1428395A (en) * 2001-12-24 2003-07-09 长春科润光电子材料科技有限公司 Red colour conversion material
CN101618946A (en) * 2009-07-03 2010-01-06 中南大学 Yb<3+>-doped oxyfluoride transparent microcrystal glass material and preparation method thereof
CN103803804A (en) * 2012-11-14 2014-05-21 中国科学院上海硅酸盐研究所 Nano glass ceramic up-conversion luminescent material and preparation method thereof
CN103666475A (en) * 2013-12-11 2014-03-26 昆明理工大学 Rare earth doped glass frequency conversion luminous material and preparation method thereof
CN105602566A (en) * 2016-02-29 2016-05-25 武汉理工大学 Rare earth-doped NaGdF4 upconversion nanocrystalline and preparation method thereof
CN106010536A (en) * 2016-05-26 2016-10-12 中国科学院宁波材料技术与工程研究所 Method for synthesizing monodisperse rare earth doped up-converted fluorescence nanocrystalline through microwave assistance, and product thereof and application
CN106082676A (en) * 2016-06-06 2016-11-09 中国科学院上海光学精密机械研究所 Mix the INFRARED ABSORPTION height Aluminous Silicate Glass-Ceramics of samarium, ytterbium

Also Published As

Publication number Publication date
CN106835261A (en) 2017-06-13

Similar Documents

Publication Publication Date Title
CN101370970B (en) Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics
JP5493092B2 (en) Method for producing gallium oxide single crystal and gallium oxide single crystal
CN105696078B (en) A kind of preparation method of monocrystalline lithium tantalate
CN107177884B (en) A kind of growing method and device of fluoride single crystal
EP3305948B1 (en) Apparatus for producing single crystal and method for producing single crystal
CN100434574C (en) Growth method for Yb and Cr4+ doped yttrium-aluminium garnet laser crystal
CN104962994A (en) Method for growing specific-size rare-earth-doped gallium-containing garnetite series crystal by edge-defined process
CN106521625B (en) Mix tetravalence chromium gallium oxide crystal and preparation method and application
CN106835261B (en) A kind of growing method and application thereof
Sun et al. Pulling growth technique towards rare earth single crystals
CN102838093A (en) LiGaGe2Se6 compound, LiGaGe2Se6 nonlinear optical crystals, and preparation method and application thereof
CN110331443A (en) A kind of rare earth ion doped germanate eutectic material and preparation method thereof
CN102168299B (en) Method for growing phosphorus-silicon-cadmium single crystal
CN103451730B (en) Cd4rO (BO3)3compound, Cd4rO (BO3)3optical crystal and preparation method and purposes
CN110468445A (en) Boric acid caesium barium nonlinear optical crystal and its preparation method and application
CN115341284B (en) High-concentration gradient neodymium doped gadolinium yttrium aluminum garnet laser crystal and preparation method thereof
CN102168305A (en) Synthesis method of phosphorus-silicon-cadmium polycrystal material
CN106012020B (en) Thulium ytterbium is co-doped with upconversion laser materials and preparation method using four molybdates as matrix
CN108893780A (en) A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof
CN103757689A (en) Method for casting monocrystalline silicon by inducing growth utilizing monocrystalline silicon seed and product
CN107858750A (en) A kind of Al2O3‑YAG:Ce3+The preparation method of eutectic fluorescence ceramics
CN100510205C (en) Yb-doped gadolinium germanate, lanthanum germanate and melt-method growth process thereof
CN105951176A (en) Fluxing agent lifting growing method for rare earth sesquioxide laser crystals
CN208136383U (en) A kind of compound thermal field structure of EFG technique growth gallium oxide single crystal
CN109695058A (en) Large scale Yb:YAG laser crystal heat exchange growing method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20180507

Address after: 200237 District 2319, room 69, Lane 1985, Chunshen Road, Minhang District, Shanghai 1 district.

Applicant after: Shanghai Langyan Optoelectronics Technology Co.,Ltd.

Applicant after: East China Normal University

Address before: 200237 District 2319, room 69, Lane 1985, Chunshen Road, Minhang District, Shanghai 1 district.

Applicant before: Shanghai Langyan Optoelectronics Technology Co.,Ltd.

GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20211018

Address after: Room 4001, building 21, No. 123, Lane 1165, Jindu Road, Minhang District, Shanghai 201100

Patentee after: SHANGHAI LANGYAN OPTOELECTRONICS TECHNOLOGY Co.,Ltd.

Patentee after: Chongqing Research Institute of East China Normal University

Address before: 200237 District 2319, room 69, Lane 1985, Chunshen Road, Minhang District, Shanghai 1 district.

Patentee before: SHANGHAI LANGYAN OPTOELECTRONICS TECHNOLOGY Co.,Ltd.

Patentee before: EAST CHINA NORMAL University

TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20230522

Address after: No. 2, 1st Floor, Building 1, No. 2 Huizhu Road, Yubei District, Chongqing, 401120

Patentee after: Chongqing Huapu Quantum Technology Co.,Ltd.

Address before: Room 4001, building 21, No. 123, Lane 1165, Jindu Road, Minhang District, Shanghai 201100

Patentee before: SHANGHAI LANGYAN OPTOELECTRONICS TECHNOLOGY Co.,Ltd.

Patentee before: Chongqing Research Institute of East China Normal University