DE2543752A1 - Single crystal growing crucible - made of material not wettable by melt carrying planar seed crystal on bottom - Google Patents
Single crystal growing crucible - made of material not wettable by melt carrying planar seed crystal on bottomInfo
- Publication number
- DE2543752A1 DE2543752A1 DE19752543752 DE2543752A DE2543752A1 DE 2543752 A1 DE2543752 A1 DE 2543752A1 DE 19752543752 DE19752543752 DE 19752543752 DE 2543752 A DE2543752 A DE 2543752A DE 2543752 A1 DE2543752 A1 DE 2543752A1
- Authority
- DE
- Germany
- Prior art keywords
- crucible
- melt
- seed crystal
- crystal
- single crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
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
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
-
- 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
- C30B11/04—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt
- C30B11/06—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method adding crystallising materials or reactants forming it in situ to the melt at least one but not all components of the crystal composition being added
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
"Anordnung zum Herstellen eines Einkristalls" "Arrangement for producing a single crystal"
Bei dem Bridgman-Verfahren zur Herstellung von Einkristallen wird die in einem Tiegel befindliche Schmelze längs eines Temperaturgradienten derart bewegt, daß ein Kristall vom Boden des Tiegels her in der Schmelze wächst. Dazu wird entweder bei feststehendem Tiegel der Ofen relativ zu dem Tiegel bewegt oder der Tiegel in dem Ofen vertikal abgesenkt. Damit überhaupt die Bildung eines Einkristalls möglich ist, wird der Tiegelboden konusförmig ausgebildet oder gegebenenfalls zusätzlich mit einer oberhalb der Konusspitze liegenden Einschnürung versehen. Bei vielen Materialien, wie z.B. Galliumarsenid, Eisenoxid oder Calcium-Wolframat, wird jedoch kein einheitlicher Einkristall erhalten, sondern es bilden sich nur polykristalline Bereiche aus. Das bekannte Verfahren würde sich durch Verwendung eines Impfkristalls wesentlich verbessern lassen. Offenbar führte bisher jedoch die Halterung eines Impfkristalls vor Beginn des Wachstums in der Schmelze zu erheblichen Schwierigkeiten.In the Bridgman process for the production of single crystals the melt located in a crucible along a temperature gradient in this way moves that a crystal grows from the bottom of the crucible in the melt. In addition the furnace is either moved relative to the crucible while the crucible is stationary, or the crucible in the furnace is lowered vertically. With it at all the formation of a single crystal is possible, the crucible bottom is designed to be conical or, if necessary, additionally provided with a constriction above the cone tip. With many materials, such as gallium arsenide, iron oxide or calcium tungstate, however, does not become more uniform Received single crystal, but only polycrystalline areas are formed. That known methods would be significantly improved by using a seed crystal permit. Apparently, however, the holding of a seed crystal before the start has so far led the growth in the melt leads to considerable difficulties.
Die Erfindung verfolgt daher den Zweck, das Bridgman-Verfahren so auszugestalten, daß das Kristallwachstum von einem Keimkristall ausgeht. Insbesondere liegt hier die aufgabe zugrunde, eine Anordnung verfügbar zu machen, die eine präzise und einfache Halterung eines scheibenförmigen Einkristalls ermöglicht.The invention therefore has the purpose, the Bridgman method so to design that the crystal growth starts from a seed crystal. In particular the underlying task here is to make an arrangement available that is precise and enables easy holding of a disk-shaped single crystal.
Diese Aufgabe wird gemäß der Erfindung dadurch gelöst, daß sich am Boden des Tiegels eine oder mehrere Öffnungen befinden, über denen am Tiegelboden ein flächenhafter Keimkristall liegt, daß der Tiegel aus einem Material besteht, das von der Schmelze nicht benetzt wird, und daß der Außenraum des Tiegels unter Unterdruck steht.This object is achieved according to the invention in that on Bottom of the crucible one or more openings are located above those on the crucible bottom there is a planar seed crystal that the crucible is made of a material that is not wetted by the melt, and that the outer space of the crucible is below There is negative pressure.
Nach einer bevorzugten Ausgestaltung der Erfindung besteht der Tiegel aus glasartiger Kohle, deren Oberfläche von keinem der zur Anwendung kommenden Materialien praktisch benetzt wird. Der glasartige Kohlenstoff ist eine spezielle Art undurchlässiger Kohlenstoff-Formkörper. Er zeigt ein glasartiges Aussehen und weist die Vor- und Nachteile von Kohlenstoff und Glas auf. Die Formkörper aus glasartigem KohlenstG»f lassen sich mit einem hohen Reinheitsgrad herstellen.According to a preferred embodiment of the invention, there is the crucible made of vitreous carbon, the surface of which is not made from any of the materials used is practically wetted. The vitreous carbon is a special kind of impermeable carbon Carbon molded body. It shows a glass-like appearance and has the advantages and Disadvantages of carbon and glass. The moldings made of vitreous carbon G »f can be produced with a high degree of purity.
Zur Herstellung dient ein organisches Polymeres, wie z.B.An organic polymer, such as e.g.
Furanharz, Phenolharz oder Styrolharz, das in einer inerten Atmosphäre auf Temperaturen zwischen 1000 und 2000 °C erhitzt wird, wodurch eine Umwandlung in den glasartigen Kohlenstoff stattfindet.Furan resin, phenolic resin or styrene resin that is in an inert atmosphere is heated to temperatures between 1000 and 2000 ° C, causing a conversion takes place in the glassy carbon.
Eine Weiterbildung der Erfindung besteht darin, daß für die Schmelze eine induktive Beheizung vorgesehen ist. Auf diese Weise läßt es sich erreichen, daß der Keimkristall unterhalb der Schmelze vor Beginn des Wachstums bestehen bleibt. Diese Maßnahme läßt sich dadurch ergänzen oder ersetzen, daß unterhalb des Tiegelbodens ein Wärmeleitkörper vorgesehen ist.A further development of the invention is that for the melt inductive heating is provided. In this way it can be achieved that the seed crystal remains below the melt before growth begins. This measure can be supplemented or replaced by the fact that below the crucible bottom a heat conducting body is provided.
Wenn dieser aus einem porösen Material besteht, das von der Schmelze nicht benetzt wird, z.B. Graphit, kann er gleichzeitig den Tiegelboden bilden.If this consists of a porous material that is melted by the melt is not wetted, e.g. graphite, it can also form the bottom of the crucible.
Das Wesen der Erfindung soll anhand zweier Figuren näher erläutert werden. In den Figuren sind gleiche Teile mit den gleichen Bezugszeichen versehen.The essence of the invention will be explained in more detail with reference to two figures will. In the figures, the same parts are provided with the same reference numerals.
In einem Tiegel (1) befindet sich die Schmelze (2), während am Tiegelboden eine Öffnung (3) vorgesehen ist, über welcher der Keimkristall (4) liegt. Zur Beheizung der Schmelze ist eine Induktionsspule vorgesehen. Aus Gründen der Ubersichtlichkeit wurden die weiteren Bestandteile der Ziehapparaturs wie z.B. eine Vorrichtung zum Absenken der Anordnung, nicht dargestellt. Es soll jedoch insbesondere darauf hingewiesen werden, daß sich die in der Figur dargestellte Tiegelanoffönung in einem evakuierbaren Gefäß befindet oder zumindest im Bereich der Öffnung (3) evakuierbar ist. Auf diese Weise kann die zwischen dem Impfkristall und der Auflagefläche des Tiegelbodens befindliche tuft über die Öffnung (3) entweichen. Da der Tiegel aus einem Material besteht, dessen erfläche von der Schmelze nicht benetzt wird, kann diese nicht zwischen den Keimkristall und den Tiegelboden laufen. Selbst wenn der Kristall spezifisch leichter als die schmelze ist, wird der Keimkristall sicher am Tiegelboden gehalten. Durch vorsichtiges Einjustieren wird vor der Kristallabscheidung zunächst die Schmelze gebildet, ohne daß der lmpfkristall sich auflöst. Es ist darauf zu achten, daß der Temperaturgradient an der Grenzfläche zwischen Keimkristall und 3chmelze möglichst groß ist. Dazu kann gegebenenfalls zusätzlich ein Wärmeleitkörper (6) am Tiegelboden angebracht werden, der mit einer Längsbohrung versehen ist, um die durch djC oeffnung (3) entweichende tuft durchzulassen.The melt (2) is in a crucible (1), while at the bottom of the crucible an opening (3) is provided over which the seed crystal (4) lies. For heating the melt is an induction coil is provided. Because of The other components of the drawing apparatus such as a Device for lowering the arrangement, not shown. However, it is particularly intended it should be noted that the Tiegelanoffönung shown in the figure located in an evacuable vessel or at least in the area of the opening (3) can be evacuated. In this way, the between the seed crystal and the support surface The tuft in the bottom of the crucible can escape through the opening (3). Because the crucible consists of a material whose surface is not wetted by the melt, this cannot run between the seed crystal and the bottom of the crucible. Even if If the crystal is specifically lighter than the melt, the seed crystal will be safe held at the bottom of the pan. Carefully adjust before the crystal separation initially the melt is formed without the seed crystal dissolving. It's on it to ensure that the temperature gradient at the interface between the seed crystal and 3melt is as large as possible. For this purpose, a heat-conducting body can optionally also be used (6) be attached to the crucible bottom, which is provided with a longitudinal bore to to let the tuft escaping through the djC opening (3) through.
Bei dem Ausführungsbeispiel nach Fig.2 besteht der Wärmeleitkörper (6) aus einem porösen Material und bildet gleichzeitig den Tiegelboden. In diesem Fall können die Öffnung im Tiegelboden und die Längsbohrung im Wärmeleitkörper entfallen. Der Unterdruck am Tiegelboden bildet sich über die Poren des Wärmeleitkörpers aus.In the embodiment according to FIG. 2, there is a heat conducting body (6) made of a porous material and at the same time forms the bottom of the crucible. In this In this case, the opening in the crucible bottom and the longitudinal bore in the heat conducting body can be omitted. The negative pressure at the bottom of the crucible is created through the pores of the heat conducting body.
Die Durchführung des Verfahrens soll anhand eines Beispiel, und zwar Galliumarsenid, erläutert werden. Der Tiegel (1) wird mittels der Induktionsspule (5) so erhitzt, daß die Schmelze (2) eine Temperatur oberhalb des Schmelzpunktes (12380C) annimmt, der Keimkristall (4) aber nicht aufschmilzt.The implementation of the procedure should be based on an example, namely Gallium arsenide. The crucible (1) is made by means of the induction coil (5) heated so that the melt (2) has a temperature above the melting point (12380C) assumes, but the seed crystal (4) does not melt.
Dazu muß sich die iegelunterseite so in einem Temperaturgradienten befinden, daß die Schmelzisotherme gerade in Höhe der Kristalloberkante liegt. Um eine Zersetzung der Schmelze zu vermeiden, befindet sich die gesamte Anordnung in einem abgeschlossenen Gefäß, in den mit einem Arsenreservoir bei ca. 610 °C der Gleichgewichtsdruck über geschmolzenem Galliumarsenid (0,97 at) aufrechterhalten wird. Nun wird die gekante Anordnung langsam abgesenkt, so daß die Schmelze in Bereiche niedrigerer temperatur gelangt und kontrolliert erstarr. Durch die Vorgabe des Keimkristalls (4) wird erreicht, daß sich ein Einkristall bildet. Alternativ kann auch die induktionsspule nach oben verschoben werden, um die gleiche Wirkung zu erzielen.For this purpose, the underside of the bar must be in a temperature gradient located that the melting isotherm is just in height the top edge of the crystal lies. In order to avoid decomposition of the melt, the entire arrangement is in place in a closed vessel with an arsenic reservoir at approx. 610 ° C Maintain equilibrium pressure over molten gallium arsenide (0.97 at) will. Now the edged arrangement is slowly lowered so that the melt in areas reaches a lower temperature and solidifies in a controlled manner. By specifying the seed crystal (4) A single crystal is made to form. Alternatively, the induction coil moved up to achieve the same effect.
Claims (6)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19752543752 DE2543752B2 (en) | 1975-10-01 | 1975-10-01 | Method and apparatus for producing a single crystal |
JP11842476A JPS5243786A (en) | 1975-10-01 | 1976-10-01 | Apparatus for making sigle crystals |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19752543752 DE2543752B2 (en) | 1975-10-01 | 1975-10-01 | Method and apparatus for producing a single crystal |
Publications (2)
Publication Number | Publication Date |
---|---|
DE2543752A1 true DE2543752A1 (en) | 1977-04-07 |
DE2543752B2 DE2543752B2 (en) | 1979-03-15 |
Family
ID=5957931
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19752543752 Withdrawn DE2543752B2 (en) | 1975-10-01 | 1975-10-01 | Method and apparatus for producing a single crystal |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE2543752B2 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4224100A (en) * | 1978-06-16 | 1980-09-23 | Litton Systems, Inc. | Method and apparatus for making crystals |
EP0517251A1 (en) * | 1991-06-07 | 1992-12-09 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
FR2853913A1 (en) * | 2003-04-17 | 2004-10-22 | Apollon Solar | Crucible for a device for fabrication of a block of crystalline material by controlled crystallisation, with a bottom transparent and walls opaque to infrared radiation |
EP1460153A3 (en) * | 1999-08-02 | 2005-04-20 | Sumitomo Electric Industries, Ltd. | Crystal growth vessel and crystal growth method |
FR2895749A1 (en) * | 2006-01-04 | 2007-07-06 | Apollon Solar Soc Par Actions | Device for producing block of crystalline material, comprises heat source and cooling system to establish thermal gradient in crystallization crucible, silica plates arranged around induction turn, and removable felt |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3026661C2 (en) * | 1980-07-14 | 1983-11-24 | Aleksandr Ivanovič Vladimir Gridnev | Device for growing single crystals from multi-component alloys |
-
1975
- 1975-10-01 DE DE19752543752 patent/DE2543752B2/en not_active Withdrawn
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4224100A (en) * | 1978-06-16 | 1980-09-23 | Litton Systems, Inc. | Method and apparatus for making crystals |
EP0517251A1 (en) * | 1991-06-07 | 1992-12-09 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
US5342475A (en) * | 1991-06-07 | 1994-08-30 | The Furukawa Electric Co., Ltd. | Method of growing single crystal of compound semiconductor |
EP1460153A3 (en) * | 1999-08-02 | 2005-04-20 | Sumitomo Electric Industries, Ltd. | Crystal growth vessel and crystal growth method |
FR2853913A1 (en) * | 2003-04-17 | 2004-10-22 | Apollon Solar | Crucible for a device for fabrication of a block of crystalline material by controlled crystallisation, with a bottom transparent and walls opaque to infrared radiation |
WO2004094704A2 (en) * | 2003-04-17 | 2004-11-04 | Apollon Solar | Crucible for a device used for the production of a block of crystalline material, and production method |
WO2004094704A3 (en) * | 2003-04-17 | 2004-12-16 | Apollon Solar | Crucible for a device used for the production of a block of crystalline material, and production method |
US7442255B2 (en) | 2003-04-17 | 2008-10-28 | Apollon Solar | Crucible for a device for producing a block of crystalline material and method for producing same |
FR2895749A1 (en) * | 2006-01-04 | 2007-07-06 | Apollon Solar Soc Par Actions | Device for producing block of crystalline material, comprises heat source and cooling system to establish thermal gradient in crystallization crucible, silica plates arranged around induction turn, and removable felt |
WO2007077305A1 (en) * | 2006-01-04 | 2007-07-12 | Apollon Solar | Device and process for producing a block of crystalline material |
Also Published As
Publication number | Publication date |
---|---|
DE2543752B2 (en) | 1979-03-15 |
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Legal Events
Date | Code | Title | Description |
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BI | Miscellaneous see part 2 | ||
BHJ | Nonpayment of the annual fee |