WO2001068956A1 - Dispositif et procede de cristallogenese - Google Patents
Dispositif et procede de cristallogenese Download PDFInfo
- Publication number
- WO2001068956A1 WO2001068956A1 PCT/FR2001/000708 FR0100708W WO0168956A1 WO 2001068956 A1 WO2001068956 A1 WO 2001068956A1 FR 0100708 W FR0100708 W FR 0100708W WO 0168956 A1 WO0168956 A1 WO 0168956A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- crucible
- crystal
- liquid
- heating means
- bulb
- Prior art date
Links
Classifications
-
- 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
- C30B11/003—Heating or cooling of the melt or the crystallised material
-
- 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
-
- 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
- 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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
Definitions
- This invention relates to a device and a method of crystallogenesis, in which a liquefied body of the composition of the crystal to be formed is enclosed in a crucible whose wall it wets and left to solidify in the presence of a germ having the structure crystal to create, so that this structure is reproduced by the body as it solidifies.
- a liquefied body of the composition of the crystal to be formed is enclosed in a crucible whose wall it wets and left to solidify in the presence of a germ having the structure crystal to create, so that this structure is reproduced by the body as it solidifies.
- an ingot of the body is deposited in the solid state in the crucible and it is liquefied in slices by a mobile heating means along the crucible away from the germ: the body gradually solidifies from of the germ, from which it still takes the crystalline structure.
- the original body thus transformed into crystal is then recovered by opening the crucible.
- French patent 2,757,184 which constitutes the closest known prior art, teaches that the solidification of the crystal causes certain difficulties since its coefficient of contraction is different from that of the crucible when it cools, which produces mechanical stresses, defects in the crystals and sometimes a rupture of the crucible, even if it contracts less than the crystal, since it adheres to it.
- This patent also teaches that a solution can be found by producing a higher gas pressure. in a bottom part of the crucible, where the crystal forms, only in a top part of the crucible, which overhangs the liquid and is also occupied by gas.
- This overpressure automatically produces a contraction of the section of the crystal at the time of its solidification, and therefore a clearance between the crystal and the crucible, which rises with the level of the crystal-liquid interface as the solidification progresses.
- This invention constitutes a perectioning of the previous one: if the known process makes it possible to obtain the stated objectives, it has certain drawbacks due to the existence of pipes leading to the two extreme regions of the crucible and making it possible to establish the difference of desired pressure.
- An essential object of the invention is therefore to do without the gas circuit without giving up the beneficial effect of the pressure difference between the two parts of the crucible.
- a closed crucible but fitted with a gas pocket, called a bulb heated by a particular and adjustable means that allows the temperature of the gas to be changed at will.
- the bulb communicates with the bottom part of the crucible and there establishes the desired overpressure by heating its contents.
- a pressure setting is therefore replaced by a temperature setting, which is easier to accomplish in practice.
- a visual observation of the solidification, and in particular of the crystal-liquid interface makes it possible to ensure the good quality of the overpressure without resorting to a sensor.
- the body which is the object of crystallogenesis comprises a liquid portion 1 surmounting a crystal 2 solidified in a closed crucible 3, of cylindrical shape and erect or inclined.
- the volume of the crucible 3 unoccupied by the liquid 1 and the crystal 2 is filled with a neutral gas, which does not react with the sample.
- the bottom region of the crucible 3 is occupied by a bulb 4 of this gas which makes it possible to apply a pressure difference between the bottom region of the crucible 3 and a top region 10 overhanging the liquid 1 and also filled with neutral gas, since the liquid 1 wets the wall of the crucible 3, while the resulting crystal 2 of a contraction to solidification is separated from this wall by a clearance.
- a heating device comprises three ovens 7; 8 and 9 superimposed, surrounding the crucible 3 and separated by insulating layers 11 and 12.
- the first two ovens 7 and 8 are usual in the art and make it possible to carry out a Brigdman solidification process, the upper oven 7 being kept at a temperature higher than that of the middle oven 8 and the interface between the crystal 2 and the liquid 1 being located at the border between the ovens 7 and 8.
- the lower oven 9 is assigned to the heating of the gas in the bulb 4 and to the pressure adjustment by varying the temperature.
- the gas pressure in the top region 10 adjusts to the volume and temperature conditions there, but an overpressure is maintained in the bottom region of the crucible due to - stronger heating of the contents of the bulb 4
- the sufficiency of this overpressure can be verified by examining the shape of the meniscus 6 formed by the liquid 1 at the point of its connection with the crystal 2: a concave meniscus will be proof of sufficient overpressure.
- the observation means used can be an optical fiber 5 passing locally through the insulating layer 11.
- the lower oven 9 is adjusted to make the heating which it produces more or less intense depending on the shape of the meniscus 6.
- the reference 13 designates a labyrinth seal composed of baffles which impose a sinuous path on the gas flows between the bulb 4 and the bottom region of the crucible 3 which is adjacent to the crystal 2, in order to thwart the heat exchanges between these two volumes without affecting the communication of pressures.
- the growth of a single crystal of CdTe 10 m long and 5 cm in diameter was carried out according to the Brigdman method.
- the crucible 3 was made of transparent silica glass and a monocrystalline seed with a diameter very slightly smaller than that of the crucible was placed under the load to be solidified.
- the vapor pressure of the liquid was 1.5 atmospheres in the top region 10, which was brought to a temperature of about 1150 ° C while the vapor pressure at the meniscus 6 was from an atmosphere at the CdTe melting temperature of 1100 ° C.
- the pressure in the bulb 4 should therefore ensure and the pressure of 1.5 atmosphere in the top region 10 and the overpressure of the bottom region of the crucible 3 to form the contraction of the crystal 2 and the meniscus 6. From the 0.4 atmosphere argon had been blown into crucible 3 before sealing it. Under these conditions, the bulb 4 was heated to 1200 ° C. using the lower oven 9 to operate the device correctly.
- the process of the invention is compatible with the presence of an upper ingot to be liquefied and then solidified.
- the ovens 7, 8 and 9 are movable along the crucible 3, the 2-liquid crystal interface 1 remaining at the height of the insulating layer 11 and the optical fiber 5, which allows to solidify.
- the oven 9 is designed to remain at the level of the bulb 4; he can comprise stepped portions in turn put into service when they pass in front of the bulb 4. It should also be noted that the bulb 4 could remain stationary and be heated by an oven separate from the furnaces for heating the body to be solidified; it would then be in communication with the crucible 3 by a deformable piping.
Landscapes
- 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)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2001567831A JP2003527297A (ja) | 2000-03-10 | 2001-03-09 | 結晶成長装置及び方法 |
EP01913972A EP1261760A1 (fr) | 2000-03-10 | 2001-03-09 | Dispositif et procede de cristallogenese |
US10/204,402 US6652647B2 (en) | 2000-03-10 | 2001-03-09 | Crystal growth device and method |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR00/03118 | 2000-03-10 | ||
FR0003118A FR2806100B1 (fr) | 2000-03-10 | 2000-03-10 | Dispositif et procede de cristallogenese |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001068956A1 true WO2001068956A1 (fr) | 2001-09-20 |
Family
ID=8847967
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2001/000708 WO2001068956A1 (fr) | 2000-03-10 | 2001-03-09 | Dispositif et procede de cristallogenese |
Country Status (5)
Country | Link |
---|---|
US (1) | US6652647B2 (fr) |
EP (1) | EP1261760A1 (fr) |
JP (1) | JP2003527297A (fr) |
FR (1) | FR2806100B1 (fr) |
WO (1) | WO2001068956A1 (fr) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2865740B1 (fr) | 2004-01-30 | 2007-06-22 | Centre Nat Rech Scient | Procede et dispositif de fabrication de monocristaux |
KR100712139B1 (ko) | 2006-05-01 | 2007-05-09 | 임항준 | 브릿지만 공정을 이용한 단결정 생성장치 및 생성방법 |
FR2927910B1 (fr) * | 2008-02-27 | 2011-06-17 | Centre Nat Rech Scient | Procede de cristallogenese d'un materiau electriquement conducteur a l'etat fondu. |
US9109299B1 (en) * | 2011-03-30 | 2015-08-18 | CapeSym, Inc. | Solidification of high quality alloy semiconductors |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4764350A (en) * | 1986-10-08 | 1988-08-16 | The United States Of America As Represented By The Secretary Of The Air Force | Method and apparatus for synthesizing a single crystal of indium phosphide |
US5037621A (en) * | 1989-11-09 | 1991-08-06 | The United States Of America As Represented By The Secretary Of The Army | System for the in-situ visualization of a solid liquid interface during crystal growth |
JPH0442888A (ja) * | 1990-06-08 | 1992-02-13 | Nikko Kyodo Co Ltd | 結晶成長装置 |
EP0565415A2 (fr) * | 1992-04-06 | 1993-10-13 | Alcatel | Procédé de fabrication d'un lingot en oxyde supraconducteur à haute température critique |
FR2757184A1 (fr) * | 1996-12-12 | 1998-06-19 | Commissariat Energie Atomique | Dispositif et procede de cristallogenese |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69934643T2 (de) * | 1998-03-31 | 2007-10-25 | Nippon Mining & Metals Co., Ltd. | Verfahren zur herstellung eines einkristalls mit halbleitender zusammensetzung |
JP3631063B2 (ja) * | 1998-10-21 | 2005-03-23 | キヤノン株式会社 | フッ化物の精製方法及びフッ化物結晶の製造方法 |
US6210605B1 (en) * | 1999-07-26 | 2001-04-03 | General Electric Company | Mn2+ activated green emitting SrAL12O19 luminiscent material |
-
2000
- 2000-03-10 FR FR0003118A patent/FR2806100B1/fr not_active Expired - Fee Related
-
2001
- 2001-03-09 EP EP01913972A patent/EP1261760A1/fr not_active Withdrawn
- 2001-03-09 JP JP2001567831A patent/JP2003527297A/ja not_active Withdrawn
- 2001-03-09 WO PCT/FR2001/000708 patent/WO2001068956A1/fr active Application Filing
- 2001-03-09 US US10/204,402 patent/US6652647B2/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4764350A (en) * | 1986-10-08 | 1988-08-16 | The United States Of America As Represented By The Secretary Of The Air Force | Method and apparatus for synthesizing a single crystal of indium phosphide |
US5037621A (en) * | 1989-11-09 | 1991-08-06 | The United States Of America As Represented By The Secretary Of The Army | System for the in-situ visualization of a solid liquid interface during crystal growth |
JPH0442888A (ja) * | 1990-06-08 | 1992-02-13 | Nikko Kyodo Co Ltd | 結晶成長装置 |
EP0565415A2 (fr) * | 1992-04-06 | 1993-10-13 | Alcatel | Procédé de fabrication d'un lingot en oxyde supraconducteur à haute température critique |
FR2757184A1 (fr) * | 1996-12-12 | 1998-06-19 | Commissariat Energie Atomique | Dispositif et procede de cristallogenese |
Non-Patent Citations (1)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 016, no. 219 (C - 0943) 22 May 1992 (1992-05-22) * |
Also Published As
Publication number | Publication date |
---|---|
US20030019421A1 (en) | 2003-01-30 |
FR2806100A1 (fr) | 2001-09-14 |
EP1261760A1 (fr) | 2002-12-04 |
FR2806100B1 (fr) | 2002-09-20 |
US6652647B2 (en) | 2003-11-25 |
JP2003527297A (ja) | 2003-09-16 |
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