CN207944167U - Czochralski method CeAlO3Crystal growing apparatus - Google Patents
Czochralski method CeAlO3Crystal growing apparatus Download PDFInfo
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- CN207944167U CN207944167U CN201820786777.9U CN201820786777U CN207944167U CN 207944167 U CN207944167 U CN 207944167U CN 201820786777 U CN201820786777 U CN 201820786777U CN 207944167 U CN207944167 U CN 207944167U
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- insulation cover
- insulation
- barrel
- cealo
- double
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000009413 insulation Methods 0.000 claims abstract description 75
- 239000013078 crystal Substances 0.000 claims abstract description 70
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 17
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005485 electric heating Methods 0.000 claims abstract description 14
- 230000006698 induction Effects 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 14
- 239000010453 quartz Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 244000144985 peep Species 0.000 claims description 7
- 239000003063 flame retardant Substances 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract description 3
- 229910052684 Cerium Inorganic materials 0.000 description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 7
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 7
- VXLGWCOZCKOULK-UHFFFAOYSA-K aluminum;cerium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Al].[Ce+3] VXLGWCOZCKOULK-UHFFFAOYSA-K 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010583 slow cooling Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 2
- 230000000994 depressogenic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 229910002637 Pr6O11 Inorganic materials 0.000 description 1
- -1 cerium aluminates Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model discloses a kind of czochralski method CeAlO3Crystal growing apparatus, include insulation cover and insulation barrel in lifting furnace, wherein, sealing forms burner hearth between the insulation cover and insulation barrel, Iridium Crucible is equipped in the insulation barrel, the Iridium Crucible is externally provided with induction coil and is heated, the insulation cover is the insulation cover of double-layer structure, the thickness range of the insulation cover of the double-layer structure is 30~50mm, in the middle cavity for imbedding double-layer heat insulation cover at the top of the insulation barrel and Iridium Crucible, it is provided with electric heating leaf in the insulation cover of the double-layer structure and forms superposition thermal field structure, thermal insulation cover is arranged in the top of the insulation cover of the double-layer structure, opening introduces lifting rod on the thermal insulation cover.Czochralski method CeAlO provided by the utility model3Crystal growing apparatus, stability is good, can effectively avoid the attenuation problem of conventional fluorescent powder, and conversion art is with a wide range of applications in flicker and fluorescence.
Description
Technical field
The utility model is related to a kind of high-temp oxide crystal grower more particularly to a kind of czochralski method cerium aluminates or dilute
Soil doping aluminic acid cerium crystal grower.
Background technology
Aluminic acid cerium crystal category cubic crystal structure, can be applied to LED fluorescent materials, avoid traditional LED fluorescent powder performance
Attenuation problem.The blue light that the efficient InGaN/GaN bases blue-ray LED of making generally use of white light LEDs is sent out excites Ce:YAG fluorescence
Powder obtains yellow light, and the yellow light inspired forms white light with remaining blue light.But find Ce during use:YAG fluorescent powder has
Apparent relaxation phenomenon：Apparent using decaying after 6000 hours, End of Life was generally reached at 1.5~20,000 hours, and (light decay reaches
50%).Therefore, how to ensure that the cerium aluminate prepared or rear-earth-doped cerium aluminate crystal stability are good, avoid traditional Ce:YAG is glimmering
The attenuation problem of light powder is most important.
In addition, crystal needs certain temperature difference to create crystal structure condition, existing crystal during growth
Growth furnace generally uses squirrel-cage heater, and power steps up, to prevent the temperature change of crystal growing process
It is too fast, defect is generated, crystal quality is influenced.But squirrel-cage heater, when under powered, temperature is also to reduce simultaneously,
It is not easily formed effective temperature gradient distribution.Therefore, existing structure is slowly to rise formation temperature by lifting rod traction crystal
Gradient is spent, crystal growth condition is created.It is not only complicated, and control difficult.
Utility model content
The technical problem to be solved by the utility model is to provide a kind of czochralski method CeAlO3 crystal growing apparatus, stability
It is good, the attenuation problem of conventional fluorescent powder can be effectively avoided, conversion art is with a wide range of applications in flicker and fluorescence.
The utility model is to solve above-mentioned technical problem and the technical solution adopted is that provide a kind of czochralski method CeAlO3It is brilliant
Body grower includes insulation cover and insulation barrel in lifting furnace, wherein seal shape between the insulation cover and insulation barrel
At burner hearth, Iridium Crucible is equipped in the insulation barrel, the Iridium Crucible is externally provided with induction coil and is heated, the insulation cover
Thickness range for the insulation cover of double-layer structure, the insulation cover of the double-layer structure is 30~50mm, the insulation barrel and iraurite
In the middle cavity for imbedding double-layer heat insulation cover at the top of crucible, it is provided with electric heating leaf in the insulation cover of the double-layer structure and is formed
It is superimposed thermal field structure, thermal insulation cover is arranged in the top of the insulation cover of the double-layer structure, and being open to introduce on the thermal insulation cover carries
Pull rod.
Above-mentioned czochralski method CeAlO3Crystal growing apparatus, wherein on the insulation cover towards at oblique upper through setting
It is in 45 degree of angles with horizontal direction to have peep hole, the peep hole.
Above-mentioned czochralski method CeAlO3Crystal growing apparatus, wherein be equipped between insulation barrel on the inside of the induction coil
The bottom of quartz barrel, the quartz barrel is mounted on by pallet and holder in lifting furnace, is filled out between the quartz barrel and insulation barrel
It is husky filled with heat preservation.
Above-mentioned czochralski method CeAlO3Crystal growing apparatus, wherein the husky heat preservation is that zirconium oxide heat preservation is husky, the pallet
Material be aluminium oxide or zirconium oxide.
Above-mentioned czochralski method CeAlO3Crystal growing apparatus, wherein the transverse height of the burner hearth is less than longitudinally wide, institute
The aspect ratio for stating burner hearth is 3~5, and temperature gradient variation is 15~20 DEG C/centimetre.
Above-mentioned czochralski method CeAlO3Crystal growing apparatus, wherein the electric heating leaf is S type corrugated plates, the electric heating
The terminals of leaf are pierced by thermal insulation cover, and the terminals of the electric heating leaf and the contact position of thermal insulation cover are equipped with fire-retardant ring, institute
Fire-retardant ring is stated to be entwined by steel band and expanded graphite tape alternation.
The utility model comparison prior art has following advantageous effect：Czochralski method CeAlO provided by the utility model3It is brilliant
Body grower, stability is good, can effectively avoid the attenuation problem of conventional fluorescent powder, the conversion art tool in flicker and fluorescence
Have wide practical use.
Description of the drawings
Fig. 1 is the utility model czochralski method CeAlO3Crystal growing apparatus structural schematic diagram.
In figure：
1 thermal insulation cover, 2 insulation barrel, 3 insulation cover
4 induction coil, 5 Iridium Crucible, 6 peep hole
7 lifting rods 8 keep the temperature husky 9 quartz barrels
10 seed crystal, 11 pallet, 12 holder
13 melt, 14 crystal, 15 electric heating leaf
Specific implementation mode
The utility model will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the utility model czochralski method CeAlO3Crystal growing apparatus structural schematic diagram.
Refer to Fig. 1, czochralski method CeAlO provided by the utility model3Crystal growing apparatus includes in lifting furnace
Insulation cover 3 and insulation barrel 2, wherein sealing forms burner hearth between the insulation cover 3 and insulation barrel 2, is equipped in the insulation barrel 2
Iridium Crucible 5, the Iridium Crucible 5 are externally provided with induction coil 4 and are heated, and the insulation cover is the insulation cover of double-layer structure,
The thickness range of the insulation cover 3 of the double-layer structure is 30~50mm, and the top of the insulation barrel 2 and Iridium Crucible 5 is imbedded double
In the middle cavity of layer insulation cover, it is provided with electric heating leaf 15 in the insulation cover of the double-layer structure and forms superposition thermal field structure,
Temperature gradient variation can be preferably controlled, the top of the insulation cover 3 is arranged thermal insulation cover 1, is open on the thermal insulation cover 1
Introduce lifting rod 7.
Czochralski method CeAlO provided by the utility model3Crystal growing apparatus, towards passing through at oblique upper on the insulation cover 3
It wears and is equipped with peep hole 6, the peep hole 6 is in 45 degree of angles with horizontal direction.The inside of the induction coil 4 and insulation barrel 2 it
Between be equipped with quartz barrel 9, the bottom of the quartz barrel 9 is mounted on by pallet 11 and holder 12 in lifting furnace, 9 He of the quartz barrel
Filled with heat preservation sand 8 between insulation barrel 2.
Czochralski method CeAlO3 crystal growing apparatus provided by the utility model, the heat preservation sand 8 is husky for zirconium oxide heat preservation, institute
The material for stating pallet 11 is aluminium oxide or zirconium oxide.The transverse height of the burner hearth be less than it is longitudinally wide, the burner hearth it is vertical
Horizontal ratio is 3~5, and temperature gradient variation is 15~20 DEG C/centimetre.The material of the insulation cover 3 and insulation barrel 2 is zirconium oxide.Institute
It is S type corrugated plates to state electric heating leaf 15, and the terminals of the electric heating leaf 15 are pierced by thermal insulation cover 1, the electric heating leaf 15
The contact position of terminals and thermal insulation cover 1 is equipped with fire-retardant ring (not shown), and the fire-retardant ring is by steel band and expanded graphite tape alternation
It is entwined, to ensure sealing effect.
Czochralski method CeAlO3 crystal growing apparatus provided by the utility model, control is using steps are as follows：
S1：Dry raw material is taken, is pressed into material pie after mixing, carries out pre-burning synthesis；
S2：Sintering block is packed into Iridium Crucible, is reloaded into lifting furnace；
S3：After installing seed crystal on lifting rod, seals burner hearth and be filled with inert gas after vacuumizing, temperature increasing for melting materials is formed
Melt, and constant temperature is kept；
S4：Using seed crystal seeding, using Czochralski grown technology controlling and process pull rate and crystal rotation；Wait for that crystal growth is complete
Cheng Hou, slow cooling take out crystal.
The utility model is directed to high-temp oxide crystal, has better oxidation resistance using Iridium Crucible 5, can grow
Such as YAG, GGG, LAO, LSAT, LYSO, the high-temp oxide crystals such as LSO.
Embodiment 1：Grow aluminic acid cerium crystal
According to molar ratio CeO2:A12O3=2:1 weighs the raw material for the drying that purity is 99.99%, is uniformly mixed,
The pressure of 100MPa depresses to 80 × 40mm of Φ3Material cake, 1500 DEG C of pre-burnings synthesize 10 hours；Φ 90 during block is fitted into will be sintered
×70mm3Iridium Crucible 5 in, and be packed into lifting furnace, seed crystal 10 is CeAlO3Seed crystal, melt 13 are CeAlO3Melt, it is brilliant
Body 14 is CeAlO3Crystal.The CeAlO in [111] direction is installed on lifting rod3Then seed crystal seals burner hearth and vacuumizing and (is better than
6×10-3Pa), high-purity N is filled with after2Gas, temperature increasing for melting materials；At melt, constant temperature 2 hours after expecting all to melt；It is given birth to using czochralski method
Long technique, pull rate are 2 mm hrs, 12 revs/min of crystal rotation.After the completion of crystal growth, slow cooling takes after 40 hours
Go out crystal, grows 50 × 80mm of Φ3Transparent complete CeAlO3Crystal.
Embodiment 2：Sm adulterates aluminic acid cerium crystal
Selection Re is Sm：Sm in molar ratio2O3:CeO2:A12O3=0.05:1.9:1 weighs the drying that purity is 99.99%
Raw material is uniformly mixed, 80 × 40mm of Φ is depressed in the pressure of 100MPa3Material cake, 1500 DEG C of pre-burnings synthesize 10 hours；It will burn
90 × 70mm of Φ during caking material is fitted into3Iridium Crucible 5 in, and be packed into lifting furnace, seed crystal 10 is CeAlO3Seed crystal, melt 13
To mix Sm cerium aluminate melts, crystal 14 is to mix Sm aluminic acid cerium crystals.The CeAlO in [111] direction is installed on lifting rod3Seed crystal,
Then it seals burner hearth and vacuumizes and (be better than 6 × 10-3Pa), high-purity N is filled with after2Gas, temperature increasing for melting materials；The Cheng Rong after expecting all to melt
Body, constant temperature 2 hours；Using Czochralski grown technique, pull rate is 1 mm hr, 12 revs/min of crystal rotation.Crystal growth
After the completion, slow cooling takes out crystal after 48 hours, has grown 50 × 60mm of Φ3Transparent complete Sm0.05:Ce0.95AlO3
Crystal.
Embodiment 3：Pr adulterates aluminic acid cerium crystal
Selection Re is Pr：According to molar ratio Pr6O11:CeO2:A12O3=0.01:1.94:1 weighs purity as 99.99%
Dry raw material is uniformly mixed, 80 × 40mm of Φ is depressed in the pressure of 100MPa3Material cake, 1500 DEG C of pre-burnings synthesis 10 is small
When；90 × 70mm of Φ during block is fitted into will be sintered3Iridium Crucible 5 in, and be packed into lifting furnace, seed crystal 10 is CeAlO3Seed crystal,
Melt 13 is to mix Pr cerium aluminate melts, and crystal 14 is to mix Pr aluminic acid cerium crystals.The CeAlO in [111] direction is installed on lifting rod3
Then seed crystal seals burner hearth and vacuumizes (better than 6 × 10-3Pa), high-purity N is filled with after2Gas, temperature increasing for melting materials；It waits expecting whole fusings
Afterwards at melt, constant temperature 2 hours；Using Czochralski grown technique, pull rate is 0.8 mm hr, 10 revs/min of crystal rotation.
After the completion of crystal growth, slow cooling takes out crystal after 48 hours, has grown 50 × 60mm of Φ3It is transparent complete
Pr0.03Ce0.97AlO3Crystal.
Although the utility model is disclosed as above with preferred embodiment, so it is not limited to the utility model, any
Those skilled in the art, without departing from the spirit and scope of the utility model, when can make a little modification and it is perfect, therefore this
The protection domain of utility model, which is worked as, is subject to what claims were defined.
Claims (6)
1. a kind of czochralski method CeAlO3Crystal growing apparatus includes insulation cover (3) and insulation barrel (2) in lifting furnace, spy
Sign is, is sealed between the insulation cover (3) and insulation barrel (2) and forms burner hearth, Iridium Crucible is equipped in the insulation barrel (2)
(5), the Iridium Crucible (5) is externally provided with induction coil (4) and is heated, and the insulation cover (3) is the insulation cover of double-layer structure,
The thickness range of the insulation cover of the double-layer structure is 30~50mm, is imbedded at the top of the insulation barrel (2) and Iridium Crucible (5)
In the middle cavity of double-layer heat insulation cover, it is provided with electric heating leaf (15) in the insulation cover of the double-layer structure and forms superposition thermal field knot
Thermal insulation cover (1) is arranged in the top of structure, the insulation cover (3), and opening introduces lifting rod (7) on the thermal insulation cover (1).
2. czochralski method CeAlO as described in claim 13Crystal growing apparatus, which is characterized in that direction on the insulation cover (3)
Peep hole (6) is provided through at oblique upper, the peep hole (6) is in 45 degree of angles with horizontal direction.
3. czochralski method CeAlO as described in claim 13Crystal growing apparatus, which is characterized in that on the inside of the induction coil (4)
Quartz barrel (9) is equipped between insulation barrel (2), the bottom of the quartz barrel (9) is mounted on by pallet (11) and holder (12)
It is husky (8) filled with heat preservation between the quartz barrel (9) and insulation barrel (2) in lifting furnace.
4. czochralski method CeAlO as claimed in claim 33Crystal growing apparatus, which is characterized in that the heat preservation husky (8) is oxidation
Zirconium heat preservation is husky, and the material of the pallet (11) is aluminium oxide or zirconium oxide.
5. czochralski method CeAlO as described in claim 13Crystal growing apparatus, which is characterized in that the transverse height of the burner hearth
Less than longitudinally wide, the aspect ratio of the burner hearth is 3~5, and temperature gradient variation is 15~20 DEG C/centimetre.
6. czochralski method CeAlO as described in claim 13Crystal growing apparatus, which is characterized in that the electric heating leaf (15) is S
The terminals of type corrugated plate, the electric heating leaf (15) are pierced by thermal insulation cover (1), the terminals of the electric heating leaf (15) and guarantor
The contact position of warm lid (1) is equipped with fire-retardant ring, and the fire-retardant ring is entwined by steel band and expanded graphite tape alternation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820786777.9U CN207944167U (en) | 2018-05-24 | 2018-05-24 | Czochralski method CeAlO3Crystal growing apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820786777.9U CN207944167U (en) | 2018-05-24 | 2018-05-24 | Czochralski method CeAlO3Crystal growing apparatus |
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| Publication Number | Publication Date |
|---|---|
| CN207944167U true CN207944167U (en) | 2018-10-09 |
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| CN (1) | CN207944167U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115874268A (en) * | 2022-12-15 | 2023-03-31 | 中国科学院上海光学精密机械研究所 | Thermal field structure for inhibiting gallium oxide volatilization |
-
2018
- 2018-05-24 CN CN201820786777.9U patent/CN207944167U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115874268A (en) * | 2022-12-15 | 2023-03-31 | 中国科学院上海光学精密机械研究所 | Thermal field structure for inhibiting gallium oxide volatilization |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200604 Address after: 200120 building 7, no.1-42, Lane 83, Hongxiang North Road, Wanxiang Town, Pudong New Area, Shanghai Patentee after: Shanghai Xi Xin Semiconductor Technology Co.,Ltd. Address before: 200237 room 602, 25 Lane 700, Luo Cheng Road, Xuhui District, Shanghai. Patentee before: Cai Yifan |
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| TR01 | Transfer of patent right |