CN108060456A - The Bridgman-Stockbarger method of beryllium aluminate crystal - Google Patents
The Bridgman-Stockbarger method of beryllium aluminate crystal Download PDFInfo
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- CN108060456A CN108060456A CN201711319598.0A CN201711319598A CN108060456A CN 108060456 A CN108060456 A CN 108060456A CN 201711319598 A CN201711319598 A CN 201711319598A CN 108060456 A CN108060456 A CN 108060456A
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- beryllium
- beryllium aluminate
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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
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/002—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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
- C30B11/02—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method without using solvents
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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 invention belongs to technical field of single crystal growth, disclose a kind of method using Bridgman-Stockbarge method for growing beryllium aluminate crystal.By raw material A l2O3With BeO according to stoichiometric ratio weighing, it is uniformly mixed, briquetting；When pre-sintering 8~12 is small under 1200~1350 DEG C of furnace temperature, through solid state reaction kinetics beryllium aluminate polycrystalline component.The beryllium aluminate seed crystal for being orientated definite is placed in the seed slot of crucible bottom, synthetic polycrystalline component is reloaded into, screws crucible cover, then crucible is placed in descent method crystal growing furnace；It vacuumizes, treats that vacuum degree reaches 1 × 10‑3During Pa, high-purity Ar is filled with as protective atmosphere；Heating is melted at 1870~1950 DEG C at the top of polycrystal raw material and seed crystal, and the control of growth interface temperature gradient is controlled in 10~40 DEG C/cm, dropping speed of the crucible in 0.5~10mm/h.The shape of beryllium aluminate crystal and size are easy to control in the present invention, avoid pollution of the volatilization to environment of beryllium oxide in melt, and more crucibles can be used and grow beryllium aluminate crystal simultaneously, and growth efficiency is high, is conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of methods using Bridgman-Stockbarge method for growing beryllium aluminate crystal, belong to crystal technique neck
Domain.
Background technology
Beryllium aluminate crystal (chemical formula BeAl2O4), 1870 DEG C of fusing point belongs to rhombic system, lattice constantBeAl2O4Crystal is a kind of excellent phosphate laser host crystal material.Swash
Light host crystal material is core and the basis of Development of Laser Technology, and act has been played in each critical stage of Development of Laser Technology
The effect of sufficient weight.At this stage, yttrium-aluminium-garnet (YAG), Yttrium Orthovanadate (YVO4), sapphire (Al2O3) it is still most prestigious to swash
Light host crystal.BeAl2O4Crystal is a kind of phosphate laser host crystal material with very big potentiality, as its physical and chemical performance of matrix
It has been more than YAG crystal, has mixed the beryllium aluminate (Cr of chromium:BeAl2O4) laser characteristics of laser crystal has been more than ruby (Cr:Al2O3)
Laser crystal, but BeAl2O4Crystal application range is far from, and YAG crystal is extensive, this key factor is：(1)BeAl2O4Crystal
Difficulty is grown greatly, it is necessary to harsher process conditions.Due to BeAl2O4The melt of crystal has very big viscosity, is growing
Easily cause cracking in journey, it is uneven that scattering point, colour band, growth striation, dopant ion concentration distribution easily occurs in the crystal of acquisition
Deng some column defects, this has severely impacted the laser activity of crystal；(2) in growth BeAl2O4During crystal, due to having in raw material
Toxic very strong Be elements, BeO is evaporate into environment in crystal growing process, and the body and environment of scientific research personnel can be made
Into very big harm, so this product with very big market and economic benefit also fails to obtain commercial development.
Application rotates the terraced method of temperature and hangs down Chinese patent (grant number CN1062318C and grant number CN101407402B) respectively
Straight static temperature gradients method successfully grows jewel rank admixture BeAl2O4Crystal, but laser crystalline substance is also not achieved in crystal quality
Body standard, make crystal be limited to laser in terms of application.Chinese patent (publication number CN1824847A) is revolved using variable speed crucible
Turn Czochralski grown Cr:BeAl2O4Crystal can improve the uniformity of crystal bath component using variable speed crucible rotation, but raw
Long Cr:BeAl2O4Crystal still can not be fully solved the defects of wrappage in crystal growing process, while using czochralski method
It can not solve the volatilization of BeO in melt this technical barrier.Russ P (RU2315134C1) grows aluminic acid using kyropoulos
Beryllium crystal, but this method cycle is longer, is unfavorable for industrialized production.
Traditional Bridgman-Stockbarge method for growing crystal (such as grant number CN101280456B and grant number CN10138940B) is not
By the way of close crucible, this can not solve the problems, such as that highly toxic volatile matter volatilization damages to human body and environment.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, a kind of BeAl is proposed2O4The Bridgman-Stockbarger method of crystal
Growing method screws crucible cover sealed crucible, can inhibit the volatilization of BeO in melt, makes melt more uniform, and obtained crystal swashs
Optical property is excellent；It also avoids BeO in melt and evaporate into that crucible is outer to damage to human body and environment.And it can grow simultaneously
The BeAl that one or more specification shape is different, crystallographic direction is different2O4Crystal improves the growth efficiency of crystal.
The technical solution of the present invention is as follows：
The Bridgman-Stockbarger method of beryllium aluminate crystal, feature are：This method comprises the following steps：
1. initial feed Al2O3With BeO according to stoichiometric ratio Al2O3：BeO=1:1 weighing is uniformly mixed and presses and forms
Powder agglomates；
2. the powder agglomates under 1200~1350 DEG C of furnace temperature pre-sintering 8~12 it is small when, through solid state reaction kinetics beryllium aluminate
Polycrystalline component；
3. the beryllium aluminate seed crystal of fixed orientation is put into crucible bottom seed slot, the beryllium aluminate for then 2. synthesizing step is more
Brilliant component is put into crucible, and screws crucible cover sealed crucible；
It 4. crucible is placed in descent method for growing stove, vacuumizes, treats that vacuum degree reaches at least 1 × 10-3During Pa, it is filled with high-purity
Ar is as protective atmosphere；
5. heating makes Control for Kiln Temperature at 1870~1950 DEG C, inoculation, growth, growth interface temperature gradient are controlled 10~40
DEG C/cm, dropping speed of the crucible control is in 0.5~10mm/h.
Further, the beryllium aluminate crystal includes beryllium aluminate host crystal and admixture beryllium aluminate (such as incorporation Cr3+、Ti4 +、V5+、Fe3+Plasma) crystal.
Further, one of described raw material BeO can use Be (OH)2Or BeCO3Substitution, the Doped ions (Cr3 +、Ti4+、V5+、Fe3+Deng) can be these ions oxide (such as Cr2O3、Ti2O3、V2O5、Fe2O3Deng) or carbonate and hydrogen
Oxide etc., all material purities are all higher than 99.9%.
Further, the crucible can be Iridium Crucible, molybdenum crucible, tungsten crucible etc., and crucible is furnished with crucible cover.
Further, crucible can be single hole or porous structure, crucible shape can be cylindrical, square column type or other
Polygon, the crystal shape of growth depend on the shape of crucible, can piece beryllium aluminate crystal of a secondary growth or once life simultaneously
Long different shape, different size beryllium aluminate crystals.
Further, the beryllium aluminate seed crystal in the definite direction can be<001>、<010>Or/and<100>Direction seed
Crystalline substance, and the beryllium aluminate crystal of different directions can be grown in same stove.
Compared with prior art, the device have the advantages that：
The present invention with power is constant, thermal field is more stable compared with the terraced method of temperature, in crystal growing process, can effective control group
Divide volatilization, crystal perfection is good, high yield rate, crystalline size and shape are easier to control, and temperature gradient of solid-liquid interface I subtracts
Few crystal cleavage etc..In addition, this method process equipment is simple and convenient to operate, low energy consumption, these are all conducive to industrialized production.
Present invention method terraced with temperature and kyropoulos growth BeAl2O4Crystal phase ratio, advantage are listed in table 1.
1 present invention of table method terraced with temperature, kyropoulos growth BeAl2O4The comparison of crystal
Specific embodiment
With reference to embodiment, the invention will be further described, but should not be limited the scope of the invention with this.
Embodiment 1：By the Al of 99.9% purity2O3With BeO according to stoichiometric ratio Al2O3：BeO=1:1 weighing, mixing
Uniformly, briquetting, the synthesised polycrystalline component when 1200 DEG C of solid phase reactions 12 are small；Then orientation is selected<001>BeAl2O4Seed crystal is put
Crucible is packed into the seed slot of cylindrical molybdenum crucible bottom, then by the polycrystalline component of synthesis, screws crucible cover sealed crucible；By earthenware
Crucible is placed in descent method crystal growing furnace, is vacuumized, and treats that vacuum degree reaches 1 × 10-3During Pa, high-purity Ar is filled with as protection gas
Atmosphere；1900 DEG C are warming up to by melting sources in crucible and entering stove position by adjusting crucible melts seed crystal top, growth interface
Temperature gradient is controlled in 40 DEG C/cm or so, and declining crucible with the speed of 1mm/h carries out crystal growth.It can obtain complete, internal
Superior in quality cylindric BeAl2O4Crystal.
Embodiment 2：By the Al of 99.9% purity2O3, BeO and Cr2O3According to stoichiometric ratio weighing, it is uniformly mixed, pressure
Block.Admixture Cr2O3And BeO and Al2O3Dosage calculated according to following reaction equation：
(1-x)Al2O3+xCr2O3+BeO→BeAl2-xCrxO4(wherein x is incorporation Cr2O3Molar concentration)
By pressure caking synthesised polycrystalline component when 1350 DEG C of solid phase reactions 8 are small；Then orientation is selected<001>BeAl2O4Seed
Crystalline substance is placed in the seed slot of rectangular shaped post tungsten crucible bottom, then the polycrystalline component of synthesis is packed into crucible, screws crucible cover sealing earthenware
Crucible；Crucible is placed in descent method crystal growing furnace, is vacuumized, treats that vacuum degree reaches 1 × 10-3During Pa, high-purity Ar conduct is filled with
Protective atmosphere；1950 DEG C are warming up to by melting sources in crucible and entering stove position by adjusting crucible melts seed crystal top, it is raw
Long interface temperature gradient is controlled in 20 DEG C/cm or so, and declining crucible with the speed of 10mm/h carries out crystal growth.It can obtain complete
, the rectangular column shape that internal soundness is excellent<001>Mix the BeAl of Cr elements in direction2-xCrxO4Laser crystal.
Embodiment 3：By the Al of 99.9% purity2O3, BeO and Ti2O3According to stoichiometric ratio weighing, it is uniformly mixed, pressure
Block.Admixture Ti2O3And BeO and Al2O3Dosage calculated according to following reaction equation：
(1-x)Al2O3+xTi2O3+BeO→BeAl2-xTixO4(wherein x is incorporation Ti2O3Molar concentration)
By pressure caking synthesised polycrystalline component when 1300 DEG C of solid phase reactions 10 are small；Then orientation is selected<010>With<001>'s
BeAl2O4Each two of seed crystal, is respectively placed in the seed slot of molybdenum crucible bottom, and crucible uses four pore structures, and wherein holes is cylinder
Shape, in addition holes is rectangular shaped post, then the polycrystalline component of synthesis is packed into crucible, screws crucible cover sealed crucible；Crucible is put
It in descent method crystal growing furnace, vacuumizes, treats that vacuum degree reaches 1 × 10-3During Pa, high-purity Ar is filled with as protective atmosphere；It rises
Temperature is to 1910 DEG C by melting sources in crucible and entering stove position by adjusting crucible melts seed crystal top, growth interface temperature ladder
Degree is controlled in 15 DEG C/cm or so, and declining crucible with the speed of 5mm/h carries out crystal growth.2 root long flat columns, 2 can be obtained simultaneously
The cylindric BeAl for mixing Ti complete, internal soundness is excellent of root2-xTixO4Laser crystal.
Finally need what is illustrated, the foregoing is merely the embodiment of the present invention, not thereby limit right model of the invention
It encloses.It is clear that associated change any to the embodiment or change that those skilled in the art are made, all will not
Beyond the design of the present invention and the protection domain of appended claims.
Claims (7)
1. the Bridgman-Stockbarger method of beryllium aluminate crystal, it is characterised in that：This method comprises the following steps：
1. initial feed Al2O3With BeO according to stoichiometric ratio Al2O3：BeO=1:1 weighing is uniformly mixed and presses and forms powder agglomates；
2. the powder agglomates under 1200~1350 DEG C of furnace temperature pre-sintering 8~12 it is small when, through solid state reaction kinetics beryllium aluminate polycrystalline
Component；
3. the beryllium aluminate seed crystal of fixed orientation is put into crucible bottom seed slot, the beryllium aluminate polycrystalline group for then 2. synthesizing step
Divide and be put into crucible, and screw crucible cover sealed crucible；
It 4. crucible is placed in descent method for growing stove, vacuumizes, treats that vacuum degree reaches at least 1 × 10-3During Pa, high-purity Ar work is filled with
For protective atmosphere；
5. heating make Control for Kiln Temperature at 1870~1950 DEG C, inoculation, growth, growth interface temperature gradient control 10~40 DEG C/
Cm, dropping speed of the crucible are controlled in 0.5~10mm/h.
2. the Bridgman-Stockbarger method of beryllium aluminate crystal according to claim 1, it is characterised in that：The aluminic acid
Beryllium crystal is beryllium aluminate host crystal or admixture beryllium aluminate crystal.
3. the Bridgman-Stockbarger method of beryllium aluminate crystal according to claim 2, it is characterised in that：The admixture
Beryllium aluminate crystal is incorporation Cr3+、Ti4+、V5+Or Fe3+The beryllium aluminate crystal of ion.
4. the Bridgman-Stockbarger method of beryllium aluminate crystal described in claim 1, it is characterised in that：The initial feed
BeO can use Be (OH)2Or BeCO3Substitution, the Doped ions Cr3+、Ti4+、V5+Or Fe3+It is the oxide of these ions
Cr2O3、Ti2O3、V2O5Or Fe2O3Or the carbonate or hydroxide of these ions, the purity of the initial feed are equal
More than 99.9%.
5. the Bridgman-Stockbarger method of beryllium aluminate crystal described in claim 1, it is characterised in that：The crucible is iraurite
Crucible, molybdenum crucible or tungsten crucible, the crucible are furnished with crucible cover.
6. the Bridgman-Stockbarger method of the beryllium aluminate crystal described in claim 1 or 5, it is characterised in that：The crucible is
Single hole or porous structure, crucible shape are cylindrical, square column type or other polygons, and the crystal shape of growth depends on crucible
Shape, can piece beryllium aluminate crystal of a secondary growth or once simultaneously grow different shape, various sizes of beryllium aluminate crystal.
7. the Bridgman-Stockbarger method of beryllium aluminate crystal described in claim 1, it is characterised in that：The definite direction
Beryllium aluminate seed crystal be<001>、<010>Or/and<100>Direction seed crystal, and the aluminium of different directions can be grown in same stove
Sour beryllium crystal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711319598.0A CN108060456A (en) | 2017-12-12 | 2017-12-12 | The Bridgman-Stockbarger method of beryllium aluminate crystal |
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| CN201711319598.0A CN108060456A (en) | 2017-12-12 | 2017-12-12 | The Bridgman-Stockbarger method of beryllium aluminate crystal |
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| CN201711319598.0A Withdrawn CN108060456A (en) | 2017-12-12 | 2017-12-12 | The Bridgman-Stockbarger method of beryllium aluminate crystal |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997853A (en) * | 1974-11-29 | 1976-12-14 | Allied Chemical Corporation | Chromium-doped beryllium aluminate lasers |
| JPS546900A (en) * | 1977-06-17 | 1979-01-19 | Seiko Epson Corp | Production of clean beryl single crystal |
| US4621065A (en) * | 1983-09-24 | 1986-11-04 | Kyocera Corporation | Chrysoberyl cat's-eye synthetic single crystal |
| CN1477241A (en) * | 2003-07-11 | 2004-02-25 | 中国科学院上海光学精密机械研究所 | Growth method of magnesium aluminate spinel crystal |
| CN101280459A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method of lanthanum aluminate crystal |
| CN101407402A (en) * | 2008-10-28 | 2009-04-15 | 宁波大学 | Beryllium aluminate crystal substrate color changing gem, and preparation and growth apparatus thereof |
-
2017
- 2017-12-12 CN CN201711319598.0A patent/CN108060456A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3997853A (en) * | 1974-11-29 | 1976-12-14 | Allied Chemical Corporation | Chromium-doped beryllium aluminate lasers |
| JPS546900A (en) * | 1977-06-17 | 1979-01-19 | Seiko Epson Corp | Production of clean beryl single crystal |
| US4621065A (en) * | 1983-09-24 | 1986-11-04 | Kyocera Corporation | Chrysoberyl cat's-eye synthetic single crystal |
| CN1477241A (en) * | 2003-07-11 | 2004-02-25 | 中国科学院上海光学精密机械研究所 | Growth method of magnesium aluminate spinel crystal |
| CN101280459A (en) * | 2007-12-28 | 2008-10-08 | 上海晶生实业有限公司 | Growing method of lanthanum aluminate crystal |
| CN101407402A (en) * | 2008-10-28 | 2009-04-15 | 宁波大学 | Beryllium aluminate crystal substrate color changing gem, and preparation and growth apparatus thereof |
Non-Patent Citations (1)
| Title |
|---|
| 尚世铉等编: "《近代物理实验技术（II）》", 30 June 1993 * |
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Application publication date: 20180522 |