CN106119965A - The preparation method of Er doping LuAG crystal - Google Patents
The preparation method of Er doping LuAG crystal Download PDFInfo
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- CN106119965A CN106119965A CN201610729260.1A CN201610729260A CN106119965A CN 106119965 A CN106119965 A CN 106119965A CN 201610729260 A CN201610729260 A CN 201610729260A CN 106119965 A CN106119965 A CN 106119965A
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- thermal insulation
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/28—Complex oxides with formula A3Me5O12 wherein A is a rare earth metal and Me is Fe, Ga, Sc, Cr, Co or Al, e.g. garnets
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to the preparation method of a kind of Er doping LuAG crystal, this preparation method includes dispensing, shove charge, melt, seeding, shouldering, isometrical lifting, finish up and the step such as cooling is to control crystal growth.The preparation method of this Er doping LuAG crystal can be prevented effectively from crystal growing process the problem of Cracking produced, and can obtain diameter 20～30mm, Er:LuAG laser crystal that quality is higher, and process stabilizing, crystal becomes stove rate higher.
Description
Technical field
The present invention relates to field of photoelectric material, especially relate to the preparation method of a kind of Er doping LuAG crystal.
Background technology
LuAG crystal is cubic lattice structure, has the high (6.73g/cm of density3), molten point high (2010 DEG C), high heat conductance
(9.6W/mK), the advantage such as big, the optical isotropy of mechanical strength, can grow under smooth solid liquid interface, be readily available Gao Guang
Learn the crystal element of quality.Due to host material LuAG possess excellence optical property, opto-electronic device, near-infrared laser,
Scintillating ceramic, cathode ray are dashed forward and are all played the biggest potentiality in many fields such as light powder.
Rare earth ion Er3+?4I11/2State and4I13/2The radiation wavelength that between state, transition produces is positioned at 2.7～3 μ m,
Due to the particularity of this wavelength, this type of laser instrument has great meaning in the application of the aspects such as medical treatment, nonlinear optics and military affairs
Justice.Multinomial test result shows, mixes Er (erbium) LuAG crystal pole and promises to be the gain medium material of solid state laser, it is achieved
High power laser light exports, and the Er crystal of mixing with LuAG as host material is the most promising a kind of crystalline material.
Summary of the invention
Based on this, it is necessary to provide a kind of Er preparation method of doping LuAG crystal.
The preparation method of a kind of Er doping LuAG crystal, comprises the steps:
Dispensing: by raw material Lu2O3、Er2O3With Al2O3Constant temperature calcination 4～10 hours at 600～1000 DEG C, natural cooling
After according to preset ratio mixed configuration bed material, the bed material that will prepare loads in container, is sufficiently mixed, then by mix homogeneously
Bed material loads in mould, passes through isostatic pressing after sealing；
Melt: by the bed material of molding calcination 24～48 hours at 1000～1300 DEG C, form polycrystal material, polycrystal material is put
In crystal growing apparatus, heating makes polycrystal material fusing obtain melt, and constant temperature keeps 1～3 hour, is slowly displaced downwardly to by seed crystal
Above melt；
Seeding: treat that seed crystal enters melt, temperature to the seed crystal of regulation melt have part micro-molten time, keep temperature 1～2 hours
After start lifting；
Shouldering: shouldering Angle ambiguity at 30～45 °, pull rate 1.5～2mm/ hour, brilliant rotary speed 19～20 revs/min
Clock；
Isometrical lifting: by changing pull rate and brilliant rotary speed, use Automatic Diameter Control method of weighing, control crystal diameter
Deviation is less than 1mm, whole during, pull rate 1～1.5mm/ hour, brilliant rotary speed 17～19 revs/min；
Ending: heat up to be gradually reduced crystal diameter, the pull rate of whole epilog is 1～1.5mm/ hour, brilliant
Rotary speed is 15～17 revs/min；
Cooling, takes out crystal after being down to room temperature with the rate of temperature fall of 20～40 DEG C/h.
Wherein in an embodiment, described seed crystal is the LuAG crystal in<111>direction.
Wherein in an embodiment, described crystal growing apparatus include metallic crucible, the first thermal insulation cover, heating coil,
Thermal insulation board, the second thermal insulation cover, the 3rd thermal insulation cover, cover plate and lifting rod；Wherein, described metallic crucible is positioned at described first thermal insulation cover
In and be filled with insulation sand between described metallic crucible and described first thermal insulation cover；Described heating coil is wound on described first insulation
On cover；Described thermal insulation board is located at described metallic crucible and the top of described first thermal insulation cover, and described thermal insulation board offered crystalline substance
Mouthful；Described second thermal insulation cover and described 3rd thermal insulation cover are positioned on described thermal insulation board and described 3rd thermal insulation cover is set in described
The outside of two thermal insulation covers；Described cover plate is positioned on described second thermal insulation cover and described 3rd thermal insulation cover；Described cover plate is provided with and carries
Pulling eye, described lifting rod can pass described lifting hole, described second thermal insulation cover and described crystalline substance mouth of crossing and seed crystal is sent into described gold
Belong to crucible.
Wherein in an embodiment, described metallic crucible is Iridium Crucible.
Wherein in an embodiment, described first thermal insulation cover is ceramic thermal insulation cover or mullite thermal insulation cover.
Wherein in an embodiment, the opening of described metallic crucible flushes with the opening of described first thermal insulation cover and sets
Put.
Wherein in an embodiment, described insulation sand is zircon sand.
Wherein in an embodiment, described second thermal insulation cover is zirconium oxide thermal insulation cover.
Wherein in an embodiment, described 3rd thermal insulation cover is aluminium oxide thermal insulation cover or mullite thermal insulation cover.
Wherein in an embodiment, described cover plate is zirconium oxide plate, and described cover plate is provided with observation port.
The preparation method of above-mentioned Er doping LuAG crystal can be prevented effectively from crystal growing process the problem of Cracking produced, can
With Er doping LuAG (also known as the Er:LuAG) laser crystal that acquisition diameter 20～30mm and quality are higher, whole preparation process work
Skill problem, crystal becomes stove rate higher.
Accompanying drawing explanation
Fig. 1 is the structural representation of the crystal growing apparatus of an embodiment；
Fig. 2 is the preparation flow schematic diagram of the Er doping LuAG crystal of an embodiment.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.In accompanying drawing
Give presently preferred embodiments of the present invention.But, the present invention can realize in many different forms, however it is not limited to institute herein
The embodiment described.On the contrary, providing the purpose of these embodiments is to make the understanding to the disclosure more thorough
Comprehensively.
It should be noted that when element is referred to as " being fixed on " another element, and it can be directly on another element
Or element placed in the middle can also be there is.When an element is considered as " connection " another element, and it can be to be directly connected to
To another element or may be simultaneously present centering elements.
Unless otherwise defined, all of technology used herein and scientific terminology and the technical field belonging to the present invention
The implication that technical staff is generally understood that is identical.The term used the most in the description of the invention is intended merely to describe tool
The purpose of the embodiment of body, it is not intended that in limiting the present invention.Term as used herein "and/or" includes one or more phase
Arbitrary and all of combination of the Listed Items closed.
As it is shown in figure 1, the crystal growing apparatus 10 of an embodiment includes metallic crucible the 11, first thermal insulation cover 12, heater wire
Circle 13, after heater the 14, second thermal insulation cover the 15, the 3rd thermal insulation cover 16, cover plate 17 and lifting rod 18.
Metallic crucible 11 is positioned at the first thermal insulation cover 12.The outer wall of metallic crucible 11 (include lateral wall with diapire outside) with
Between the inwall of the first thermal insulation cover 12, there is gap, in this gap, fill completely insulation sand 19.In the present embodiment, metallic crucible 11
For Iridium Crucible.First thermal insulation cover 12 is ceramic thermal insulation cover or mullite thermal insulation cover.Insulation sand 19 is zircon sand.Metallic crucible 11
The opening of opening and the first thermal insulation cover 12 flushes and fills up insulation sand between setting, and metallic crucible 11 and the first thermal insulation cover 12
19。
Heating coil 13 is wound on the first thermal insulation cover 12, for metallic crucible 11 carries out sensing heating.
Thermal insulation board 14 is located at metallic crucible 11 and the top of the first thermal insulation cover 12.Brilliant mouth 142 was offered on thermal insulation board 14,
For passing for crystal.
Second thermal insulation cover 15 and the 3rd thermal insulation cover 16 is positioned on thermal insulation board 14 and the 3rd thermal insulation cover 16 is set in the second insulation
The outside of cover 15.In the present embodiment, the second thermal insulation cover 15 is zirconium oxide thermal insulation cover.3rd thermal insulation cover 16 is aluminium oxide thermal insulation cover
Or mullite thermal insulation cover.Use the second thermal insulation cover 15 and the 3rd thermal insulation cover 16 with the use of, be conducive to reducing radially thermal stress, with
Reduce the probability of crystal cleavage.
Cover plate 17 is positioned on the second thermal insulation cover 15 and the 3rd thermal insulation cover 16.Cover plate 17 is provided with lifting hole 172.In this enforcement
In example, cover plate 17 is zirconium oxide plate.Further, in the present embodiment, cover plate 17 is provided with observation port 174.The axle of observation port 174
To the setting axial at an acute angle with metallic crucible 11.Observation port 174 is for for detection head image checking such as CCD.
Lifting rod 18 through lifting hole the 172, second thermal insulation cover 15 and can cross brilliant mouth 142, sends into metal earthenware for seed crystal
Crucible 11.
Above-mentioned crystal growing apparatus 10 can be used for but not limit in the preparation process of Er doping LuAG crystal, raw for crystal
Long, by using this crystal growing apparatus to coordinate crystal growth condition to control, generation can be prevented effectively from crystal growing process
Problem of Cracking, crystal becomes stove rate higher.
Incorporated by reference to Fig. 1 and Fig. 2, the present embodiment additionally provides the preparation method of a kind of Er doping LuAG crystal.This preparation side
Method uses above-mentioned crystal growing apparatus 10, including dispensing, melt, seeding, shouldering, isometrical lifting, finishes up and the step such as cooling, tool
Body is as follows.
Dispensing: by raw material Lu2O3、Er2O3With Al2O3Constant temperature calcination 4～10 hours at 600～1000 DEG C, natural cooling
After according to preset ratio mixed configuration bed material, the bed material that will prepare loads in container, is sufficiently mixed, then by mix homogeneously
Bed material loads in mould, passes through isostatic pressing after sealing.
Raw material Lu2O3、Er2O3With Al2O3Preferably high-purity raw, such as 5N grade high-purity raw material etc..
Melt: by the bed material of molding calcination 24～48 hours at 1000～1300 DEG C, form polycrystal material, polycrystal material is put
In the metallic crucible 11 of crystal growing apparatus 10, heating makes polycrystal material fusing obtain melt 20, and constant temperature keeps 1～3 hour,
Seed crystal 30 is slowly displaced downwardly to above melt 20.
When heating makes polycrystal material melt, it is preferred to use high-purity nitrogen or noble gas are as protective atmosphere.
It is further preferred that in the present embodiment, seed crystal 30 is the LuAG crystal in<111>direction.Seed crystal 30 is fixed on and carries
One end of pull bar 18,
Seeding: treat that seed crystal 30 enters melt 20, temperature to the seed crystal 30 of regulation melt 20 have part micro-molten time, keep temperature
Lifting is started after 1～2 hour.
Shouldering: shouldering Angle ambiguity at 30～45 °, pull rate 1.5～2mm/ hour, brilliant rotary speed 19～20 revs/min
Clock.
Isometrical lifting: by changing pull rate and brilliant rotary speed, use Automatic Diameter Control method of weighing, control crystal 40 straight
Footpath deviation is less than 1mm, whole during, pull rate 1～1.5mm/ hour, brilliant rotary speed 17～19 revs/min.
Described Automatic Diameter Control method of weighing is to use the existing device automatically controlling crystal growth diameter, crystal growth
Quality by sensor incoming computer crystal growth software, software performs growth according to the Automatic Program set in advance and grasps
Make.
Ending: heat up to be gradually reduced crystal 40 diameter, the pull rate of whole epilog is 1～1.5mm/ hour,
Brilliant rotary speed is 15～17 revs/min.
Cooling, takes out crystal 40 after being down to room temperature with the rate of temperature fall of 20～40 DEG C/h.
When the temperature of crystal growing apparatus 10 is down to room temperature, take out crystal 40, grow a size of Ф 25 × 120mm, etc.
The heavy 300g of path length 60mm, crystalline substance, the Er:LuAG crystal that outward appearance is good, no significant defect, optical property are good, wherein mix Er atom
Concentration about 0.5%.
Frequency Induction Heating metal is preferably used with heating coil 13 during the preparation method of above-mentioned Er doping LuAG crystal
Crucible 11.
Preparation method and the crystal growing apparatus 10 of above-mentioned Er doping LuAG crystal can be prevented effectively from crystal growing process
The problem of Cracking produced, it is possible to obtain diameter 20～30mm and higher Er doping LuAG (also known as the Er:LuAG) laser of quality are brilliant
Body, whole preparation process technological problems, crystal becomes stove rate higher.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, not to above-mentioned reality
The all possible combination of each technical characteristic executed in example is all described, but, as long as the combination of these technical characteristics is not deposited
In contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that, come for those of ordinary skill in the art
Saying, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. the preparation method of an Er doping LuAG crystal, it is characterised in that comprise the steps:
Dispensing: by raw material Lu2O3、Er2O3With Al2O3Constant temperature calcination 4～10 hours at 600～1000 DEG C, press after natural cooling
According to preset ratio mixed configuration bed material, the bed material prepared is loaded in container, is sufficiently mixed, then by the bed material of mix homogeneously
Load in mould, after sealing, pass through isostatic pressing；
Melt: by the bed material of molding calcination 24～48 hours at 1000～1300 DEG C, form polycrystal material, polycrystal material is placed in crystalline substance
In bulk-growth device, heating makes polycrystal material fusing obtain melt, and constant temperature keeps 1～3 hour, and seed crystal is slowly displaced downwardly to melt
Top；
Seeding: treat that seed crystal enters melt, temperature to the seed crystal of regulation melt have part micro-molten time, keep temperature 1～open after 2 hours
Begin to lift；
Shouldering: shouldering Angle ambiguity at 30～45 °, pull rate 1.5～2mm/ hour, brilliant rotary speed 19～20 revs/min；
Isometrical lifting: by changing pull rate and brilliant rotary speed, use Automatic Diameter Control method of weighing, control crystal diameter deviation
Less than 1mm, whole during, pull rate 1～1.5mm/ hour, brilliant rotary speed 17～19 revs/min；
Ending: heat up to be gradually reduced crystal diameter, the pull rate of whole epilog is 1～1.5mm/ hour, brilliant rotating speed
Degree is 15～17 revs/min；
Cooling, takes out crystal after being down to room temperature with the rate of temperature fall of 20～40 DEG C/h.
2. the preparation method of Er doping LuAG crystal as claimed in claim 1, it is characterised in that described seed crystal is<111>side
To LuAG crystal.
3. the preparation method of Er doping LuAG crystal as claimed in claim 1 or 2, it is characterised in that described crystal growth fills
Put and include metallic crucible, the first thermal insulation cover, heating coil, thermal insulation board, the second thermal insulation cover, the 3rd thermal insulation cover, cover plate and lifting rod；
Wherein, described metallic crucible is filled with in described first thermal insulation cover and between described metallic crucible and described first thermal insulation cover
Insulation sand；Described heating coil is wound on described first thermal insulation cover；Described thermal insulation board is located at described metallic crucible and described first
The top of thermal insulation cover, described thermal insulation board offered brilliant mouth；Described second thermal insulation cover and described 3rd thermal insulation cover are positioned at described
On thermal insulation board and described 3rd thermal insulation cover is set in the outside of described second thermal insulation cover；Described cover plate is positioned at described second thermal insulation cover
And on described 3rd thermal insulation cover；Described cover plate be provided with lifting hole, described lifting rod can pass described lifting hole, described second
Seed crystal is sent into described metallic crucible by thermal insulation cover and described crystalline substance mouth of crossing.
4. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described metallic crucible is iraurite
Crucible.
5. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described first thermal insulation cover is pottery
Porcelain thermal insulation cover or mullite thermal insulation cover.
6. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that the opening of described metallic crucible
End flushes setting with the opening of described first thermal insulation cover.
7. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described insulation sand is zircon sand.
8. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described second thermal insulation cover is oxygen
Change zirconium thermal insulation cover.
9. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described 3rd thermal insulation cover is oxygen
Change aluminum thermal insulation cover or mullite thermal insulation cover.
10. the preparation method of Er doping LuAG crystal as claimed in claim 3, it is characterised in that described cover plate is zirconium oxide
Plate, and described cover plate is provided with observation port.
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|---|---|---|---|
| CN201610729260.1A CN106119965A (en) | 2016-08-25 | 2016-08-25 | The preparation method of Er doping LuAG crystal |
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| CN201610729260.1A CN106119965A (en) | 2016-08-25 | 2016-08-25 | The preparation method of Er doping LuAG crystal |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108893780A (en) * | 2018-07-19 | 2018-11-27 | 中山大学 | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof |
| WO2021031139A1 (en) * | 2019-08-21 | 2021-02-25 | 眉山博雅新材料有限公司 | Multi-component garnet-structured scintillation crystal growth method and equipment |
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| CN103074685A (en) * | 2013-02-01 | 2013-05-01 | 中山大学 | High concentration Nd-doped YAG laser crystal growth method |
| CN103370452A (en) * | 2011-02-17 | 2013-10-23 | 克莱托斯波尔公司 | Preparation of doped garnet structure single crystals with diameters of up to 500 mm |
| JP2015036349A (en) * | 2013-08-12 | 2015-02-23 | 宇部興産株式会社 | Method for manufacturing ceramic composite |
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|---|---|---|---|---|
| US20070170154A1 (en) * | 2003-06-26 | 2007-07-26 | Semiconductor Energy Laboratory Co., Ltd. | Laser irradiation apparatus, laser irradiation method, and method for manufacturing semiconductor device |
| CN1560329A (en) * | 2004-03-04 | 2005-01-05 | 上海交通大学 | Growing process of thulium doped yttrium aluminate laser crystal |
| CN103370452A (en) * | 2011-02-17 | 2013-10-23 | 克莱托斯波尔公司 | Preparation of doped garnet structure single crystals with diameters of up to 500 mm |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108893780A (en) * | 2018-07-19 | 2018-11-27 | 中山大学 | A kind of crystal growing apparatus and the double-doped LuAG crystal of a kind of Er, Yb and preparation method thereof |
| WO2021031139A1 (en) * | 2019-08-21 | 2021-02-25 | 眉山博雅新材料有限公司 | Multi-component garnet-structured scintillation crystal growth method and equipment |
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