CN109402723A - A kind of VB/VGF method crystal growth quartz ampoule and device - Google Patents
A kind of VB/VGF method crystal growth quartz ampoule and device Download PDFInfo
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- CN109402723A CN109402723A CN201811532469.4A CN201811532469A CN109402723A CN 109402723 A CN109402723 A CN 109402723A CN 201811532469 A CN201811532469 A CN 201811532469A CN 109402723 A CN109402723 A CN 109402723A
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- quartz ampoule
- quartz
- support slot
- crystal growth
- cap
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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
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
The present invention provides a kind of VB/VGF method crystal growth quartz ampoule and device, it is related to compound crystal growing technology field, the technical solution adopted is that: a kind of VB/VGF method crystal growth quartz ampoule, including quartzy tube body and quartz cap, key is, the support slot of the circumferentially arranged opening upwards in the quartz tube body top, the quartz cap are inserted into support slot, and are realized by the through-hole that lower end is arranged in and be connected to inside and outside quartz ampoule.Beneficial effect is: this VB/VGF method crystal growth quartz ampoule is simple and practical in structure, does not have to welding tube sealing, avoids " bombing " caused by pressure difference, repeats practical, saving cost；VB/VGF method crystal growth device can be directly realized by furnace body, uniformly vacuumize in quartz ampoule, subsequent to make the quartzy seal of tube by the variation of sealant heating status, ensure that crystal growth pressure.
Description
Technical field
The present invention relates to technical field of crystal growth, are to be related to a kind of VB/VGF method crystal growth stone more specifically
English pipe and device.
Background technique
VB/VGF method is one of growth high quality, the main technique technology of low dislocation crystal.Currently, mature VB/VGF
Method crystal technique is that seed crystal, dehydration boron oxide, polycrystal material are fitted into pyrolytic boron nitride (PBN) crucible, then by PBN crucible
It is attached in quartz ampoule and is loaded onto sealing cap, by vacuumizing, vacuum in quartz ampoule is extracted into required vacuum degree, then by quartz ampoule and stone
English cap is welded to sealing together, is finally putting into VGF furnace and is pyrolyzed.Wherein used quartz ampoule needs welded seal, so
And the quartz ampoule of welded seal, it on the one hand can only be disposable, it causes at high cost；On the other hand, it heated up in crystal growth
Cheng Zhong, often occur due to temperature program or be put into the conditions such as red phosphorus amount it is improper so that quartz ampoule inside and outside differential pressure be greater than quartz ampoule
The pressure born and " bombing " phenomenon occurs, cause interrupt crystal growth, quartz ampoule damage, reduce production efficiency, also make
It is wasted at cost.
Application No. is 201420795278.8 utility model patents to disclose a kind of dress of multi-element compounds polycrystal synthesis
Material container and melt processed system, including quartz ampoule and quartzy sealing cap, quartz ampoule inner hollow, an end closure, another end opening,
Quartzy sealing cap can be inserted into from the opening or that extracts is assemblied in quartz ampoule；The quartz ampoule is in close sealing or/and opens
The outer wall of mouth is equipped with the multiple grooves being recessed inwardly, and realizes the accurate positionin of quartzy sealing cap after charging, but and unresolved brilliant
Quartz ampoule pressure imbalance problem, still be easy to cause growth course to interrupt in body growth course, low efficiency.
Summary of the invention
To solve easily " bombing " damage, disposable at high cost during the growth process of existing crystal growth quartz ampoule
Technical problem, the present invention provides a kind of VB/VGF method crystal growth quartz ampoule and device is borrowed using split type quartz ampoule structure
The through-hole of junction is helped to realize inside and outside connection, and the ingenious state change by by sealant forms heating fluid-tight, thus real
Show in crystal growing process that quartz ampoule inside and outside differential pressure is adjustable in a certain range, avoided since pressure difference leads to quartz ampoule bombing,
Also make quartz ampoule reusable, reduces costs.
The technical solution adopted by the present invention is that:
A kind of VB/VGF method crystal growth quartz ampoule, including quartzy tube body and quartz cap, it is critical that on the quartz tube body
The support slot of the circumferentially arranged opening upwards in portion, the quartz cap are inserted into support slot, and real by the through-hole that lower end is arranged in
The existing inside and outside connection of quartz ampoule.
The through-hole of the quartz cap lower end is equipped with more than one.
The support slot is U-type groove or V-groove.
The heated solid particle sealant for becoming liquid and forming sealing is equipped in the support slot.
It is equipped with below the support slot and connects bakie.
The present invention also provides a kind of VB/VGF method crystal growth devices, furnace body, furnace body including being equipped with vacuum lead
Interior heater limits the crucible inside the quartz ampoule and quartz ampoule of bottom of furnace body by supporter, wraps in quartz ampoule structure
Quartzy tube body and quartz cap are included, it is critical that the support slot of the circumferentially arranged opening upwards in the quartz tube body top, support slot
Interior to be equipped with the heated solid particle sealant for becoming liquid and forming sealing, the quartz cap is inserted into support slot, and by setting
Through-hole in lower end is realized and is connected to inside and outside quartz ampoule.
The through-hole of the quartz cap lower end is equipped with more than one.
The support slot is U-type groove or V-groove.
It is equipped with below the support slot and connects bakie.
In above-mentioned technical proposal, a kind of VB/VGF method crystal growth quartz ampoule, including quartzy tube body and stone are provided first
English cap, key Design are that the support slot of the quartzy circumferentially arranged opening upwards in tube body top, the quartz cap is inserted into support slot
It is interior, and have in support slot and move up and down freedom degree, the lower end of quartz cap is equipped with through-hole structure, by through-hole structure, quartz
The inside and outside connection of pipe.
VB/VGF method crystal growth device is set in furnace body including furnace body, quartz ampoule and crucible equipped with vacuum lead
Having heaters, is used for heated quarty tube and furnace atmosphere temperature, and quartz ampoule is limited by supporter in bottom of furnace body, quartz ampoule knot
It include quartzy tube body and quartz cap in structure, crucible is arranged inside quartz ampoule, it is critical that quartzy tube body top is circumferentially arranged
The support slot of opening upwards, support slot is interior to be equipped with the heated solid particle sealant for becoming liquid and forming sealing, the quartz cap
It is inserted into support slot, and has in support slot and move up and down freedom degree, the lower end of quartz cap is equipped with through-hole structure, by through-hole
Structure, the inside and outside connection of quartz ampoule.
When carrying out crystal growth using the present apparatus, seed crystal, dehydration boron oxide and polycrystal material are sequentially placed into crucible first, and
Crucible is put into quartz ampoule, is calculated further according to pressure, temperature needed for growth technique and The Ideal-Gas Equation PV=MRT/m
Red phosphorus amount needed for quartzy tube space, the good red phosphorus of weighing and calculating are simultaneously placed into quartz ampoule.Into the support slot of quartzy tube body
Fluid-tight agent is inserted, then quartz cap is inserted into support slot, charging finishes.Charged quartz ampoule is placed in furnace body, pumping is passed through
Vacuum pipe vacuumizes, so that reaching setting vacuum degree in furnace body and in quartz ampoule, heating melts solid particle sealant all
Change, form sealing, at this time the inside and outside isolation of quartz ampoule, then increase temperature heating polycrystal material, make fusing at the top of seed crystal, it is raw to start crystal
Long-range order carries out crystal growth, after the completion of crystal growth, is annealed and obtains crystal.Solid particle sealant melts sealing
Afterwards, during reheating, when red phosphorus is greater than quartz ampoule receiving pressure by thermogenetic vapour pressure in quartz ampoule, quartz cap can be upward
It is mobile to form pressure release and quartz ampoule is avoided to burst until withstand top surface on furnace body, when quartzy overpressure is low quartz cap decline again from
And maintain pressure needed for crystal growth.
The beneficial effects of the present invention are: (1) VB/VGF method crystal growth provided by the invention is simply real with quartz ampoule structure
With without welding tube sealing, quartz ampoule inside and outside differential pressure in crystal growing process can automatically adjust in a certain range, avoid pressure
" bombing " caused by difference；(2) quartz ampoule repeats practical, saves cost；(3) by the way that solid particle sealant is arranged in support slot
And it is ingenious change to form sealing by its heating status, avoid polycrystal material loss and cause not match；(4) VB/VGF method chemical combination
Object crystal growth device can be directly realized by furnace body, uniformly vacuumize in quartz ampoule, subsequent to become by sealant heating status
Change makes the quartzy seal of tube, to guarantee its crystal growth pressure.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of VB/VGF method crystal growth quartz ampoule of the invention；
Fig. 2 is the structural schematic diagram of VB/VGF method crystal growth device of the invention；
In figure, 1, furnace body, 2, heater, 3, supporter, 4, seed crystal, 5, boron oxide, 6, polycrystal material, 7, crucible, 8, quartzy tube body,
9, support slot, 10, quartz cap, 11, upper of furnace body insulation board, 12, through-hole, 13, connect bakie, 14 be vacuum lead.
Specific embodiment
Below with specific embodiment a kind of VB/VGF method crystal growth quartz ampoule provided by the present invention will be described in detail and
The structure and application method of device, but the protection scope that the invention is not limited in any way, one of ordinary skill in the art according to
The improvement modification or similar replacement that technical solution is carried out, should all be included in the protection scope of the present invention.
Embodiment 1
A kind of VB/VGF method crystal growth quartz ampoule, including quartzy tube body 8 and quartz cap 10,8 top edge of the quartz tube body
The support slot 9 of circumferential setting opening upwards, the quartz cap 10 are inserted into support slot 9, and by the through-hole 12 that lower end is arranged in
Realize the inside and outside connection of quartz ampoule.
The present embodiment provides a kind of VB/VGF method crystal growth quartz ampoules to wrap in quartz ampoule structure referring to figure 1
Include quartzy tube body 8 and quartz cap 10, the support slot 9 of the circumferentially arranged opening upwards in quartzy 8 top of tube body, the insertion branch of quartz cap 10
It supportting in slot 9, quartz cap 10 has in support slot 9 moves up and down freedom degree, and the lower end of quartz cap is equipped with 12 structure of through-hole, by
12 structure of through-hole, quartz ampoule is inside and outside to realize pressure communication.Wherein, support slot 9 may be disposed at quartzy 8 outer surface of tube body or interior table
Face is arranged at outer surface, and 10 internal diameter of quartz cap is greater than 8 outer diameter of quartzy tube body；It is arranged in inner surface, 10 outer diameter of quartz cap is small
In quartzy 8 internal diameter of tube body, the present embodiment, support slot 9 is set to quartzy 8 outer surface of tube body, production easy to produce.
The through-hole 12 of 10 lower end of quartz cap is equipped with more than one, preferably 2,4,6,8 etc., symmetrically lays
It sets, to guarantee that all directions pressure is consistent in vacuum.
The support slot 9 is U-type groove or V-groove, i.e., the longitudal section of quartzy tube body 9 sees that support slot 9 can be U-type groove or V-type
Slot, preferably U-type groove, U-type groove bottom surface flatness is higher, is conducive to the contact with support slot 9 of quartz cap 10 and stablizes.
The heated solid particle sealant for becoming liquid and forming sealing is equipped in the support slot 9, in use, Gu
Body particulate sealant is heated to be become liquid from solid-state and forms fluid-tight, realizes the isolation inside and outside quartz ampoule, the cooperation solid of through-hole 12
Grain sealant realizes the self-sealing that quartz ampoule can uniformly vacuumize with furnace body, then realize quartz ampoule by heating, to protect
Demonstrate,prove crystal growth.
It is equipped with below the support slot 9 and connects bakie 13, overflow when melting to prevent the solid particle sealant in support slot 9 is heated
Out.
The VB/VGF method crystal growth of the present embodiment when in use, is grown in VB/VGF method compound monocrystal with quartz ampoule
It is used in furnace.
Embodiment 2
A kind of VB/VGF method crystal growth device, including being equipped with the furnace body 1 of vacuum lead 14, the heater 2 in furnace body 1,
The crucible 7 inside the quartz ampoule and quartz ampoule of 1 bottom of furnace body is limited by supporter 3, includes quartz ampoule in quartz ampoule structure
Body 8 and quartz cap 10, the support slot 9 of the circumferentially arranged opening upwards in quartz 8 top of tube body, interior be equipped with of support slot 9 are heated
Become the solid particle sealant that liquid forms sealing, the quartz cap 10 is inserted into support slot 9, and by lower end is arranged in
Through-hole 12 realizes the inside and outside connection of quartz ampoule.
VB/VGF method crystal growth device provided in this embodiment includes being equipped in apparatus structure referring to shown in attached drawing 2
Furnace body 1, quartz ampoule and the crucible 7 of vacuum lead 14, furnace body 1 is interior to be equipped with heater 3, is used for heated quarty tube and furnace atmosphere
Temperature；Quartz ampoule limits the bottom in furnace body 1 by supporter 3, includes quartzy tube body 8 and quartz cap in the structure of quartz ampoule
10, crucible 7 is arranged inside quartzy tube body 8, creative, the support slot of the circumferentially arranged opening upwards in quartzy 8 top of tube body
9, support slot 9 is interior to become the solid particle sealant of liquid formation sealing equipped with being heated, in the insertion support slot 9 of quartz cap 10, and
Have in support slot 9 and move up and down freedom degree, the lower end of quartz cap 10 is equipped with 12 structure of through-hole, by 12 structure of through-hole, stone
The inside and outside connection of English pipe.
The through-hole 12 of 10 lower end of institute's quartz cap is equipped with more than one.
The support slot 9 is U-type groove or V-groove.
It is equipped with below the support slot 9 and connects bakie 13.
When carrying out crystal growth using the present apparatus, seed crystal 4, dehydration boron oxide 5 and polycrystal material 6 are sequentially placed into crucible first
7,7 diameter of crucible is 2 inches~12 inches, and crucible 7 is put into quartz ampoule, further according to pressure, temperature needed for growth technique and
Red phosphorus amount needed for The Ideal-Gas Equation PV=MRT/m calculates quartzy tube space, the good red phosphorus of weighing and calculating are simultaneously placed into
In quartz ampoule.Quartz cap 10 is inserted into support slot 9, then solid particle sealant is inserted into the remaining space in support slot 9, Gu
The preferred boron oxide granule of body particulate sealant, charging finish.Charged quartz ampoule is placed in furnace body 1, vacuum-pumping tube is passed through
Road 14 vacuumizes, so that reaching setting vacuum degree in furnace body 1 and in quartz ampoule, heating melts solid particle sealant all,
Sealing is formed, at this time the inside and outside isolation of quartz ampoule, then increase temperature heating polycrystal material 6 and make to melt at the top of seed crystal 4, starts crystal
Growth procedure carries out crystal growth, after the completion of crystal growth, is annealed and obtains crystal.Solid particle sealant melts sealing
Afterwards, during reheating, when red phosphorus is greater than quartz ampoule receiving pressure by thermogenetic vapour pressure in quartz ampoule, quartz cap 10 can
Move up, in the present embodiment, upper of furnace body insulation board 11 be equipped in furnace body 1, when quartz cap 10 moves up maximum displacement be
Upper of furnace body insulation board 11 is withstood, quartz cap 10 is moved up to form pressure release, be burst so as to avoid quartz ampoule, quartzy overpressure
Quartz cap 10 declines to maintain pressure needed for crystal growth again when low.The present invention is for protecting VB/VGF method crystal growth stone
The structure of English pipe and device construction, not to temperature, the pressure control etc. in crystal growth, related temperature, pressure control
It can be achieved with existing furnace body, be the prior art.
To sum up, VB/VGF method crystal growth quartz ampoule provided by the invention is simple and practical in structure, and repeatable makes
With avoiding the accidental damage in crystal growing process, improve success rate, also reduce cost；VB/VGF method crystal growth
It is uniformly vacuumized with device is ingenious by solid particle sealant state change formation furnace body, in quartz ampoule, subsequent self-sealing.
Claims (9)
1. a kind of VB/VGF method crystal growth quartz ampoule, including quartzy tube body (8) and quartz cap (10), which is characterized in that institute
The support slot (9) of the circumferentially arranged opening upwards in quartzy tube body (8) top is stated, quartz cap (10) insertion support slot (9) is interior,
And the inside and outside connection of quartz ampoule is realized by the through-hole (12) that lower end is arranged in.
2. quartz ampoule according to claim 1, which is characterized in that the through-hole (12) of quartz cap (10) lower end is equipped with one
More than a.
3. quartz ampoule according to claim 1, which is characterized in that the support slot (9) is U-type groove or V-groove.
4. quartz ampoule according to claim 1 to 3, which is characterized in that be equipped with heated become in the support slot (9)
Liquid forms the solid particle sealant of sealing.
5. quartz ampoule according to claim 1 to 3, which is characterized in that be equipped with below the support slot (9) and connect bakie
(13).
6. a kind of VB/VGF method crystal growth device, including being equipped with the furnace body (1) of vacuum lead (14), in furnace body (1)
Heater (2) limits the crucible (7) inside the quartz ampoule and quartz ampoule of furnace body (1) bottom, quartz ampoule by supporter (3)
It include quartzy tube body (8) and quartz cap (10) in structure, which is characterized in that described quartzy tube body (8) top is circumferentially arranged opens
The upward support slot (9) of mouth, support slot (9) is interior to be equipped with the heated solid particle sealant for becoming liquid formation and sealing, the stone
English cap (10) is inserted into support slot (9), and realizes the inside and outside connection of quartz ampoule by the through-hole (12) that lower end is arranged in.
7. device according to claim 6, which is characterized in that the through-hole (12) of quartz cap (10) lower end is equipped with one
More than.
8. device according to claim 6, which is characterized in that the support slot (9) is U-type groove or V-groove.
9. according to device as claimed in claim 6 to 8, which is characterized in that be equipped with below the support slot (9) and connect bakie
(13).
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811532469.4A CN109402723A (en) | 2018-12-14 | 2018-12-14 | A kind of VB/VGF method crystal growth quartz ampoule and device |
| PCT/CN2019/083281 WO2020118999A1 (en) | 2018-12-14 | 2019-04-18 | Quartz tube and device for crystal growth by vb/vgf method |
| JP2020522301A JP6913430B2 (en) | 2018-12-14 | 2019-04-18 | Quartz tube and equipment for crystal growth by VB / VGF method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811532469.4A CN109402723A (en) | 2018-12-14 | 2018-12-14 | A kind of VB/VGF method crystal growth quartz ampoule and device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109402723A true CN109402723A (en) | 2019-03-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811532469.4A Pending CN109402723A (en) | 2018-12-14 | 2018-12-14 | A kind of VB/VGF method crystal growth quartz ampoule and device |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP6913430B2 (en) |
| CN (1) | CN109402723A (en) |
| WO (1) | WO2020118999A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020118999A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Quartz tube and device for crystal growth by vb/vgf method |
| CN111962139A (en) * | 2020-09-17 | 2020-11-20 | 广东先导先进材料股份有限公司 | Method for preparing gallium arsenide crystal by VGF process |
| CN113481604A (en) * | 2021-07-09 | 2021-10-08 | 武汉拓材科技有限公司 | High-purity gallium telluride polycrystal synthesis production device |
| CN115771996A (en) * | 2022-11-18 | 2023-03-10 | 云南中科鑫圆晶体材料有限公司 | Vacuum sealing and welding method of oversized-diameter quartz tube for VGF crystal growth |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114318497B (en) * | 2022-01-25 | 2024-10-01 | 洛阳市自动化研究所有限公司 | Zone melting furnace for preparing alloy crystal bar |
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- 2018-12-14 CN CN201811532469.4A patent/CN109402723A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020118999A1 (en) * | 2018-12-14 | 2020-06-18 | 中国电子科技集团公司第十三研究所 | Quartz tube and device for crystal growth by vb/vgf method |
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| CN113481604A (en) * | 2021-07-09 | 2021-10-08 | 武汉拓材科技有限公司 | High-purity gallium telluride polycrystal synthesis production device |
| CN115771996A (en) * | 2022-11-18 | 2023-03-10 | 云南中科鑫圆晶体材料有限公司 | Vacuum sealing and welding method of oversized-diameter quartz tube for VGF crystal growth |
| CN115771996B (en) * | 2022-11-18 | 2024-03-22 | 云南中科鑫圆晶体材料有限公司 | Vacuum seal welding method of oversized-diameter quartz tube for VGF crystal growth |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2021510139A (en) | 2021-04-15 |
| JP6913430B2 (en) | 2021-08-04 |
| WO2020118999A1 (en) | 2020-06-18 |
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Application publication date: 20190301 |