DE2300989A1 - PROCESS FOR GROWING CRYSTALS OF HIGH PERFECTION FROM CONVECTION-FREE MELT SUBSTANCE - Google Patents
PROCESS FOR GROWING CRYSTALS OF HIGH PERFECTION FROM CONVECTION-FREE MELT SUBSTANCEInfo
- Publication number
- DE2300989A1 DE2300989A1 DE2300989A DE2300989A DE2300989A1 DE 2300989 A1 DE2300989 A1 DE 2300989A1 DE 2300989 A DE2300989 A DE 2300989A DE 2300989 A DE2300989 A DE 2300989A DE 2300989 A1 DE2300989 A1 DE 2300989A1
- Authority
- DE
- Germany
- Prior art keywords
- medium
- liquid
- substance
- substance mass
- mass
- 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.)
- Pending
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
- C30B27/00—Single-crystal growth under a protective fluid
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/14—Heating of the melt or the crystallised materials
-
- 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
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
-
- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
-
- 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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
Description
Pat Bl/PePat Bl / Pe
Verfahren zum Züchten von Kristallen hoher Perfektion aus konvektionsfreier schmelzflüssiger SubstanzmasseProcess for growing crystals of high perfection from convection-free molten liquid Substance mass
Die Erfindung betrifft ein Verfahren zum Züchten von Kristallen aus dem Schmelzfluß, wobei die entsprechende Substanzmasse konvektionsfrei ist.The invention relates to a method for growing crystals from the melt flow, the corresponding Substance mass is free of convection.
Die Konvektion in einer Schmelze, aus der heraus Kristalle nach an sich bekannten Techniken - wie z.B. nach den Ziehmethoden von Czochralski und Nacken-Kyropoulos, den Absenkverfahren nach Bridgman und Stockbarger bzw. der Züchtung aus der Flußschmelze (Flux) mit Kühlstellen oder Keimkristallen - gezüchtet werden, ist als Ursache für viele Kristallbaufehler bekannt.Convection in a melt from which crystals emerge according to known techniques - such as the pulling methods of Czochralski and Nacken-Kyropoulos, the Lowering method according to Bridgman and Stockbarger or the cultivation from the river melt (flux) with cooling points or seed crystals - are grown is known to be the cause of many crystal defects.
Neben induktiv verursachten Konvektionsströmungen in der schmelzflüssigen Substanzmasse sind es vor allem die thermisch bedingten Konvektionsströme, die durch die unterschiedliche Dichte einzelner Schmelzbereiche innerhalb der zusammenhängenden Substanzmasse entstehen. Diese partiellen Dichteunterschiede innerhalb einer Substanzmasse führen jedoch nur dann zu Konvektionsströmungen der vorbezeichneten Art, wenn sich die Substanzmasse in einem Schwerefeld befindet.In addition to inductively caused convection currents in the molten substance mass, it is above all the thermally induced convection currents that are caused by the different Density of individual melting areas arise within the coherent substance mass. However, these partial differences in density within a substance mass only lead to convection currents of the aforementioned type when the substance mass is in a gravitational field.
Die Schwerelosigkeit läßt sich nun dadurch simulieren, daß man einen Körper bzw. ein definiertes Schmelzvolumen innerhalb eines Mediums zum Schweben bringt.Weightlessness can now be simulated by placing a body or a defined volume of enamel floating within a medium.
- Z- - Z-
409828/0627409828/0627
?' ? ' A 1 904A 1 904
4.1.19734.1.1973
Die Aufgabe der vorliegenden Erfindung ist es datier, die • für eine- perfekte Ausbildung der zu züchtenden Kristalle nachteiligen Konvektionsströmungen innerhalb einer schmelzflüssigen Substanzmasse zu unterbinden.The object of the present invention is to date the • for a perfect formation of the crystals to be grown, disadvantageous convection currents within a to prevent molten substance mass.
Diese Aufgabe wird erfindungsgemäß durch ein Verfahren gelöst, wie es in den Ansprüchen beschrieben ist. Es werden Kristalle mittels an sich bekannter Schmelzfluß-Techniken aus einer zusammenhängenden Substanzmasse gezüchtet, die in einem flüssigen Medium enthalten ist-.According to the invention, this object is achieved by a method as described in the claims. It will Crystals by means of melt flow techniques known per se grown from a coherent mass of substance contained in a liquid medium.
Dabei kann es vorteilhaft sein, wenn die Substanzmasse in dem flüssigen Medium frei schwebt. Es ist aber auch möglich, die oben genannten Techniken zum Züchten von perfekten Einkristallen aus einer schmelzflüssigen Substanzmasse dann anzuwenden, wenn letztere aufgrund von lediglich geringen Dichteunterschieden bezüglich des sie umgebenden Mediums entweder aufsteigt und somit schwimmend im Medium verbleibt, oder aber absinkt und somit auf dem Boden des das Medium enthaltenden Gefäßes ruht.It can be advantageous here if the substance mass floats freely in the liquid medium. It is also possible the above techniques for growing perfect single crystals from a molten mass of substance to be used if the latter due to only small differences in density with respect to the the surrounding medium either rises and thus remains floating in the medium, or else sinks and thus on the bottom of the vessel containing the medium rests.
Normalerweise ist das Medium so gewählt, daß es mit der sich im flüssigen und/oder im festen Zustand befindlichen Substanzmasse nicht reagiert.'Für gewisse andere Fälle - zum Beispiel bei definierten Dotier- oder Dekorier-Prozeesen - kann es aber auch zweckmäßig sein, daß das Medium so gewählt ist, daß es in definierter Weise mit der Substanzmasse reagiert. Dabei kann das Medium ausschließlich mit der flüssigen oder aber mit der festen Substanzmasse ■ reagieren. Es kann vorteilhaft sein, daß das flüssige Medium mindestens einen für die Substanzmasse bestimmten Dotier- oder Dekorierstoff enthält. Dieser kann in ionogener, molekularer oder partikularer Form in dem Medium vorhanden sein.Normally the medium is chosen so that it is in the liquid and / or in the solid state with the Substance mass does not react. For certain other cases - for example with defined doping or decorating processes - But it can also be useful that the medium is chosen so that it is in a defined way with the substance mass reacts. The medium can be used exclusively with the liquid or with the solid Substance mass ■ react. It can be advantageous that the liquid medium has at least one for the substance mass contains certain doping or decorating substance. This can be ionic, molecular or particulate Form in the medium.
409828/0627 - 3 -409828/0627 - 3 -
~ 3 ~ 3 A 1904A 1904
ΤΓΤ7ΤΨΓ3ΤΓΤ7ΤΨΓ3
Schließlich kann das Medium - entsprechend den jeweils anzuwendenden Schmelzbedingungen, wie beispielsweise Schmelzdauer, Schmelztemperatur, Schmelzmaterial - eine anorganische oder organische Flüssigkeit, Lösung oder Schmelze sein. Schmelzsysteme ohne Mischbarkeit bzw. mit Mischungslücken sind für das erfindungsgemäße Züchtungsverfahren besonders geeignet.Finally, the medium can - according to the melting conditions to be used in each case, such as, for example Melting time, melting temperature, melting material - an inorganic or organic liquid, solution or Be melt. Melt systems without miscibility or with miscibility gaps are suitable for the cultivation process according to the invention particularly suitable.
Als Beispiel für einen nach dem Züchtungsverfahren gemäß vorliegender Erfindung herstellbaren Kristall sei die Substanz Salicylsäurephenylesther (HO·C^H^·CO2*C^H-) (Salol) genannt. The substance salicylic acid phenyl ester (HO · C ^ H ^ · CO 2 * C ^ H-) (Salol) may be mentioned as an example of a crystal which can be produced by the growth process according to the present invention.
Der Schmelzpunkt dieser organischen Substanz liegt bei 43 C. Als Medium kommt Wasser in Betracht. Da die Dichte des geschmolzenen Salols bei 50 C einen Wert von 1,1553 g/cm aufweist, sinkt diese schmelzflüssige Salol-Substanzmasse in reinem H„0 auf den Boden des Gefäßes. Durch geeignete Zusätze zum Wasser-Medium könnte aber auch eine solche Dichte eingestellt werden, daß die Salol-Substanzmasse zusammenhängend schwebend im Medium verbleibt.The melting point of this organic substance is 43 C. A suitable medium is water. Because the density of the molten salol at 50 ° C. has a value of 1.1553 g / cm has, this molten Salol substance mass sinks in pure H "0 on the bottom of the vessel. By means of suitable additives to the water medium, however, such a Density can be set so that the Salol substance mass remains coherently floating in the medium.
Die schmelzflüssige Substanzmasse nimmt im Schwebezustand eine rotationssymmetrische Tröpfchenform an.The molten substance mass adopts a rotationally symmetrical droplet shape when in suspension.
Das die Substanzmasse umhüllende flüssige Medium dient gleichzeitig einer vorzugsweise allseitigen Wärmezuführung und damit der Aufrechterhaltung der einmal eingestellten Temperaturbedingungen. Die üblicherweise verwendeten Mittel für die Erzeugung und Regelung der jeweiligen optimalen Temperaturbedingungen sind hier der Einfachheit halber weggelassen worden.The liquid medium enveloping the substance mass serves at the same time to supply heat, preferably on all sides and thus the maintenance of the temperature conditions once set. The commonly used Means for generating and regulating the respective optimal temperature conditions are here for the sake of simplicity have been omitted for the sake of
Die konvektionsfreie, zusammenhängende Substanzmasse bildet somit das Reservoir für das aus ihr erfolgende Ziehen des. Kristalls.The convection-free, coherent substance mass forms thus the reservoir for pulling the crystal from it.
40 9828/06 2 7 k 40 9828/06 2 7 k
4.1.19734.1.1973
Dabei kann in bekannter Weise ein an einer drehbaren und verschiebbaren Kristallhalterung montierter Keimkristall
in die zusammenhängende Substanzmasse eingeführt werden
und danach durch kontrollierte Ortsveränderung des Kristallkeims relativ zur Substanzmasse der Züchtungsvorgang ablaufen.
A seed crystal mounted on a rotatable and displaceable crystal holder can be introduced into the coherent substance mass in a known manner
and then the growth process takes place through controlled relocation of the crystal nucleus relative to the substance mass.
409828/0627409828/0627
Claims (1)
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2300989A DE2300989A1 (en) | 1973-01-10 | 1973-01-10 | PROCESS FOR GROWING CRYSTALS OF HIGH PERFECTION FROM CONVECTION-FREE MELT SUBSTANCE |
CH1770873A CH567870A5 (en) | 1973-01-10 | 1973-12-18 | |
NL7317718A NL7317718A (en) | 1973-01-10 | 1973-12-27 | |
JP48144788A JPS4998784A (en) | 1973-01-10 | 1973-12-28 | |
GB20874A GB1427501A (en) | 1973-01-10 | 1974-01-03 | Crystal growing |
FR7400625A FR2322635A1 (en) | 1973-01-10 | 1974-01-08 | PROCESS FOR THE PRODUCTION OF HIGH PERFECTION CRYSTALS FROM A MASS OF MELTED SUBSTANCE FREE OF CONVECTION |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE2300989A DE2300989A1 (en) | 1973-01-10 | 1973-01-10 | PROCESS FOR GROWING CRYSTALS OF HIGH PERFECTION FROM CONVECTION-FREE MELT SUBSTANCE |
Publications (1)
Publication Number | Publication Date |
---|---|
DE2300989A1 true DE2300989A1 (en) | 1974-07-11 |
Family
ID=5868653
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE2300989A Pending DE2300989A1 (en) | 1973-01-10 | 1973-01-10 | PROCESS FOR GROWING CRYSTALS OF HIGH PERFECTION FROM CONVECTION-FREE MELT SUBSTANCE |
Country Status (6)
Country | Link |
---|---|
JP (1) | JPS4998784A (en) |
CH (1) | CH567870A5 (en) |
DE (1) | DE2300989A1 (en) |
FR (1) | FR2322635A1 (en) |
GB (1) | GB1427501A (en) |
NL (1) | NL7317718A (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1983003431A1 (en) * | 1982-03-30 | 1983-10-13 | Paul Otto Knischka | Gradient process for growing crystals in liquid media |
FR2549751A1 (en) * | 1983-07-29 | 1985-02-01 | Commissariat Energie Atomique | PROCESS FOR PRODUCING A MATERIAL BY MOLDING |
FR2549744A1 (en) * | 1983-07-29 | 1985-02-01 | Commissariat Energie Atomique | PROCESS FOR THE PREPARATION OF THIN OR MASSIVE METALLIC OR SEMI-METALLIC FORMS, IN PARTICULAR SILICON |
WO1991011546A1 (en) * | 1990-02-02 | 1991-08-08 | E.I. Du Pont De Nemours And Company | Doped crystalline compositions and a method for preparation thereof |
-
1973
- 1973-01-10 DE DE2300989A patent/DE2300989A1/en active Pending
- 1973-12-18 CH CH1770873A patent/CH567870A5/xx not_active IP Right Cessation
- 1973-12-27 NL NL7317718A patent/NL7317718A/xx unknown
- 1973-12-28 JP JP48144788A patent/JPS4998784A/ja active Pending
-
1974
- 1974-01-03 GB GB20874A patent/GB1427501A/en not_active Expired
- 1974-01-08 FR FR7400625A patent/FR2322635A1/en not_active Withdrawn
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1983003431A1 (en) * | 1982-03-30 | 1983-10-13 | Paul Otto Knischka | Gradient process for growing crystals in liquid media |
US4525171A (en) * | 1982-03-30 | 1985-06-25 | Knischka Rubine Gesellschaft M.B.H | Gradient process of growing crystals from liquid media |
FR2549751A1 (en) * | 1983-07-29 | 1985-02-01 | Commissariat Energie Atomique | PROCESS FOR PRODUCING A MATERIAL BY MOLDING |
FR2549744A1 (en) * | 1983-07-29 | 1985-02-01 | Commissariat Energie Atomique | PROCESS FOR THE PREPARATION OF THIN OR MASSIVE METALLIC OR SEMI-METALLIC FORMS, IN PARTICULAR SILICON |
EP0136196A1 (en) * | 1983-07-29 | 1985-04-03 | Commissariat à l'Energie Atomique | Process for making thin or massive, metallic or semimetallic objects, especially of silicium |
US4617084A (en) * | 1983-07-29 | 1986-10-14 | Commissariat A L'energie Atomique | Process for the production of metallic or semimetallic shaped elements |
WO1991011546A1 (en) * | 1990-02-02 | 1991-08-08 | E.I. Du Pont De Nemours And Company | Doped crystalline compositions and a method for preparation thereof |
Also Published As
Publication number | Publication date |
---|---|
JPS4998784A (en) | 1974-09-18 |
GB1427501A (en) | 1976-03-10 |
NL7317718A (en) | 1974-07-12 |
CH567870A5 (en) | 1975-10-15 |
FR2322635A1 (en) | 1977-04-01 |
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