DE1228235B - Process for the production of single crystal rods from silicon carbide - Google Patents
Process for the production of single crystal rods from silicon carbideInfo
- Publication number
- DE1228235B DE1228235B DES89788A DES0089788A DE1228235B DE 1228235 B DE1228235 B DE 1228235B DE S89788 A DES89788 A DE S89788A DE S0089788 A DES0089788 A DE S0089788A DE 1228235 B DE1228235 B DE 1228235B
- Authority
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- Germany
- Prior art keywords
- silicon carbide
- mixture
- compounds
- crystal
- seed 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.)
- Pending
Links
- 239000013078 crystal Substances 0.000 title claims description 21
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 20
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000000203 mixture Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000007858 starting material Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000012495 reaction gas Substances 0.000 claims description 5
- 150000004820 halides Chemical class 0.000 claims description 3
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 3
- 229910018540 Si C Inorganic materials 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 239000002019 doping agent Substances 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910003676 SiBr4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- -1 e.g. B. CH Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012433 hydrogen halide Chemical class 0.000 description 1
- 229910000039 hydrogen halide Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- AIFMYMZGQVTROK-UHFFFAOYSA-N silicon tetrabromide Chemical compound Br[Si](Br)(Br)Br AIFMYMZGQVTROK-UHFFFAOYSA-N 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/24—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only semiconductor materials not provided for in groups H01L29/16, H01L29/18, H01L29/20, H01L29/22
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/34—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies not provided for in groups H01L21/0405, H01L21/0445, H01L21/06, H01L21/16 and H01L21/18 with or without impurities, e.g. doping materials
- H01L21/46—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/428
- H01L21/479—Application of electric currents or fields, e.g. for electroforming
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
- H01S3/16—Solid materials
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Electromagnetism (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
Verfahren zum Herstellen einkristalliner Stäbe aus Siliciumcarbid Dieser Verfahren stellt eine vorteilhafte Kombination des bekannten, insbesondere zur Herstellung von Rubinen zur Anwendung kommenden Verneuilverfahrens, bei dem die feinverteilten Ausgangsmaterialien in so kleinen Mengen kontinuierlich oder schubweise auf die mittels einer Knallgasflamme hocherhitzte Spitze eines senkrecht stehenden Keimkristalls aufgebracht werden, mit dem bekannten Verfahren zum Herstellen von Siliciumcarbid in feinkristalliner Form durch Pyrolyse eines stöchiometrischen Gemisches von gasförmigen Verbindungen der Komponenten dar.Process for producing single crystal rods from silicon carbide This method represents an advantageous combination of the known, in particular for the manufacture of rubies to be used Verneuilververfahren, in which the finely divided starting materials in such small amounts continuously or in batches on the tip of a vertically heated by means of an oxyhydrogen flame standing seed crystal are applied, with the known method for manufacturing of silicon carbide in finely crystalline form by pyrolysis of a stoichiometric Mixture of gaseous compounds of the components.
Mit Hilfe des Verfahrens nach der Lehre der Erfindung lassen sich einkristalline Stäbe aus Siliciumearbid herstellen, die sich durch eine gute Kristallperfektion auszeichnen. Derartige Stäbe können sowohl zur Herstellung an sich bekannter Halbleiterbauelemente, wie Transistoren, Gleichrichter oder Fotoanordnungen als auch zur Herstellung von Lasem oder Heizleiterstäben verwendet werden.With the help of the method according to the teaching of the invention can Manufacture monocrystalline rods from silicon carbide, which are characterized by good crystal perfection distinguish. Such rods can be used both for the production of known semiconductor components, such as transistors, rectifiers or photo arrays as well as for the production of Lasem or heat conductor rods can be used.
Das beanspruchte Verfahren, bei dem ein Gemisch aus gasförmigen Verbindungen der Komponenten in Gegenwart eines Trägergases an einem Siliciumcarbid-Einkristall thermisch zersetzt wird, ist dadurch gekennzeichnet, daß man in an sich bekannter Weise die Ausgangsmaterialien im stöchiometrischen Verhältnis in kleinen Mengen kontinuierlich oder schubweise auf die mittels einer Knallgasflamme hoch erhitzte Spitze des senkrecht stehenden Keimkristalls aufbringt.The claimed method in which a mixture of gaseous compounds of the components in the presence of a carrier gas on a silicon carbide single crystal is thermally decomposed, is characterized in that one is known per se Make the starting materials in stoichiometric proportions in small amounts continuously or in batches on the highly heated by means of an oxyhydrogen flame Applies the tip of the vertically standing seed crystal.
Als Ausgangsmaterial könnenentwedergasförnüge Halogenide der Komponenten in einem Mischungsverhältnis, das der stöchiometrischen Zusammensetzung von Siliciumcarbid entspricht, verwendet werden oder aber siliciumorganische Verbindungen, die eine Si-C-Bindung im Molekül enthalten. Es hat sich gezeigt, daß sich hierfür nicht nur Substanzen wie SiC13 - CH3, SiHCI2 - CH., sondern auch solche Substanzen eignen, die außer Kohlenstoff, Silicium und Wasserstoff auch noch Sauerstoff im Molekül enthalten, wie z. B. CH,3 - S' - Cl2 - OCH,' Weiterhin sind als Ausgangsmaterialien Gemische aus Silicium-und Kohlenwasserstoffen bzw. aus den entsprechenden Halogenderivaten, wie CCIP CHCl3 oder CHBr. oder SiHC13 und SiC14 oder SiBr4, geeignet. Es ist dabei lediglich auf das Mischungsverhältnis zu achten, das auch in diesem Fall der stöchiometrischen Zusammensetzung des erwünschten Reaktionsproduktes entsprechen muß.Either gas-free halides of the components in a mixing ratio which corresponds to the stoichiometric composition of silicon carbide or organosilicon compounds which contain a Si-C bond in the molecule can be used as the starting material. It has been shown that not only substances such as SiC13 - CH3, SiHCl2 - CH., But also substances that contain oxygen in the molecule in addition to carbon, silicon and hydrogen, such as e.g. B. CH, 3 - S ' - Cl2 - OCH,' Further starting materials are mixtures of silicon and hydrocarbons or of the corresponding halogen derivatives, such as CCIP CHCl3 or CHBr. or SiHC13 and SiC14 or SiBr4, are suitable. It is only necessary to pay attention to the mixing ratio, which in this case too must correspond to the stoichiometric composition of the desired reaction product.
Als Trägergas ist Wasserstoff bevorzugt geeignet. Der Anteil der earbidbildenden Verbindungen liegt vorteilhaft in einem Bereich von 0,01 bis 60 Volumprozent im Gasgemisch.Hydrogen is preferably suitable as the carrier gas. The proportion of earbid-forming compounds is advantageously in a range from 0.01 to 60 percent by volume in the gas mixture.
Der für die Durchführung der Siliciumearbidabscheidung günstigste Druckbereich liegt zwischen 0,1 und 10 at.The most favorable pressure range for carrying out the silicon carbide deposition is between 0.1 and 10 at.
Um die für das Aufschmelzen der auf den Keimkristall gelangenden Partikeln notwendige Temperatur von etwa 1450 bis 1700' C zu erreichen, ist es vorteilhaft, eine Chlorknallgasflamme zu verwenden. In order to reach the temperature of approximately 1450 to 1700 ° C. necessary for the melting of the particles reaching the seed crystal, it is advantageous to use a chlorine oxyhydrogen flame.
Bei einer speziellen Ausführungsforin des Verfahrens gemäß der Erfindung ist vorgesehen, daß dem Reaktionsgas in bekannter Weise Dotierungsstoffe in Form gasföriniger Verbindungen, beispielsweise von Halogenverbindungen wie A1C13 oder Al-organischen Verbindungen beigefügt werden.In a special embodiment of the method according to the invention it is provided that the reaction gas in a known manner dopants in the form gaseous compounds, for example halogen compounds such as A1C13 or Al-organic compounds are added.
Nähere Einzelheiten der Erfindung gehen aus dem an Hand der Figur beschriebenen Ausführungsbeispiel hervor.Further details of the invention can be found in the figure described embodiment.
In der Figur ist eine zur Durchführung des Verfahrens gemäß der Erfindung geeignete Anordnung schematisch dargestellt.In the figure is one for carrying out the method according to the invention suitable arrangement shown schematically.
Diese Ausführungsform sieht die Verwendung einer Chlorknallgasflamrne vor. Ein an seinem unteren Ende fest eingespannter Keimkristall 1 aus Siliciumcarbid, der eine Länge von etwa 3 mm und einen Durchmesser von annähernd 1 mm besitzt, ist in einem Schutzrohr 2 aus einem hochfeuerfesten Material untergebracht. Der Kristall kann dabei durch geeignete Ausbildung der Befestigungsvorrichtung 3 nach unten abgesenkt werden. Die Zuführung des Reaktionsgasgemisches erfolgt mit Hilfe von Wasserstoff als Trägergas durch das Zuführungsrohr 4, das so ausgebildet ist, daß seine Düse 5 direkt auf die obere Spitze des Keimkristalls gerichtet ist. Durch ein weiteres Zuführungsrohr 6 wird Chlor zugeführt. Der Aufbau der Gaszuführungsvorrichtung entspricht dem Aufbau eines an sich bekannten Knallgasbrenners. Durch die bei der Verbrennung des Chlorknallgasgemisches entstehende Reaktionswärme wird an der Spitze des Keimkristalls die Zone 7 auf eine für den Einbau aus der Gasphase hinzutretender Siliciunicarbidpartikehl hinreichend hohe Temperatur, . beispielsweise 17000 C, erhitzt; die bei der Zersetzung bei der herrschenden hohen Temperatur gebildeten Si- und C-Partikeln vereinigen sich augenblicklich zu Siliciumcarbid und werden in das Gitter des Keimkristalls als SiC eingebaut. Es ist dabei darauf zu achten, daß jeweils nur so wenig Siliciumcarbid zugeführt wird, daß die Siliciumcarbidpartikeln orientiert in das Gitter eingebaut werden 'lÜönnen. Die entstehenden Restgase strömen durch das Schutzrohr nach unten ab. Der Kristall kann entweder im Laufe des Wachstums kontinuierlich nach unten abgesenkt werden oder aber periodisch um größere Strecken nach unten geführt werden. Für eine gleichmäßige Ausbildung des Einkristallstabes ist es jedoch zweckmäßig, die Absenkung kontinuierlich vorzunehmen.This embodiment provides for the use of a chlorine gas flame. A seed crystal 1 made of silicon carbide, which is firmly clamped at its lower end and has a length of approximately 3 mm and a diameter of approximately 1 mm, is accommodated in a protective tube 2 made of a highly refractory material. The crystal can be lowered down by a suitable design of the fastening device 3. The reaction gas mixture is fed in with the aid of hydrogen as the carrier gas through the feed pipe 4, which is designed so that its nozzle 5 is directed directly at the upper tip of the seed crystal. Chlorine is fed in through a further feed pipe 6. The structure of the gas supply device corresponds to the structure of an oxyhydrogen gas burner known per se. By the produced during combustion of the chlorine and hydrogen gas mixture the heat of reaction zone 7 to a kicking added for the installation from the gas phase Siliciunicarbidpartikehl sufficiently high temperature at the tip of the seed crystal. for example 17000 C, heated; the Si and C particles formed during the decomposition at the prevailing high temperature combine instantly to form silicon carbide and are incorporated into the lattice of the seed crystal as SiC. Care must be taken that only so little silicon carbide is added that the silicon carbide particles can be built into the grid in an oriented manner. The resulting residual gases flow down through the protective tube. The crystal can either be continuously lowered downwards in the course of its growth or it can be periodically moved downwards by longer distances. For a uniform formation of the single crystal rod, however, it is expedient to carry out the lowering continuously.
Das Verfahren -kann durch entsprechende Auswahl der carbidbildenden Komponenten variiert werden. Die Verwendung sfliciumorganischer Verbindungen oder aber von Gemischen aus Halogeniden oder entsprechenden Wasserstoff- bzw. Halogenwasserstoffverbindungen der carbidbildenden Substanzen führt in jedem Fall zur Bildung von Siliciumcarbid, da bei den genannten Umsetzungen die Reaktionsenthalpien stets negativ sind. Es ist hierbei nur zu beachten, daß das Mischungsverhältnis der Ausgangsmaterialien jeweils der stöchiometrischen Zusammensetzung des Siliciumcarbids entspricht und daß die Menaen des auf den Keimkristall gelangenden Materials nur gering sind, da sonst der orientierte Einbau in den Keimkristall unmöglich ist. Außerdem muß beachtet werden, daß die Strömungsgeschwindigkeit des Reaktionsgases so gewählt wird, daß die überschüssige Reaktionsenergie abgeführt wird.The process can be varied by appropriate selection of the carbide-forming components. The use of organosilicon compounds or mixtures of halides or corresponding hydrogen or hydrogen halide compounds of the carbide-forming substances always leads to the formation of silicon carbide, since the enthalpies of reaction are always negative in the reactions mentioned. It is only to be noted here that the mixing ratio of the starting materials corresponds in each case to the stoichiometric composition of the silicon carbide and that the quantities of the material reaching the seed crystal are only small, since otherwise the oriented incorporation into the seed crystal is impossible . In addition, it must be ensured that the flow rate of the reaction gas is chosen so that the excess reaction energy is dissipated.
PÜr die Verwendung von nach diesem Verfahren hergestelltem Siliciumcarbid in der Halbleitertechnik ist es vielfach notwendig, dotiertes Material zu erhalten. -Zu diesem Zweck wird dem Reaktionsgasgemisch in bekannter Weise Dotierungsmaterial in Form einer gasförmigen Verbindung, vorzugsweise eines Chlorids, zugeführt. Es besteht auch die Mög- lichkeit, dotierte Keimkristalle zu verwenden, die beispielsweise durch Sublimation hergestellt wordeiisind.For the use of silicon carbide produced by this process in semiconductor technology, it is often necessary to obtain doped material. For this purpose, doping material in the form of a gaseous compound, preferably a chloride, is added to the reaction gas mixture in a known manner. It is also possible to use doped seed crystals which have been produced, for example, by sublimation.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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DES89788A DE1228235B (en) | 1964-03-02 | 1964-03-02 | Process for the production of single crystal rods from silicon carbide |
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DES89788A DE1228235B (en) | 1964-03-02 | 1964-03-02 | Process for the production of single crystal rods from silicon carbide |
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DE1228235B true DE1228235B (en) | 1966-11-10 |
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DES89788A Pending DE1228235B (en) | 1964-03-02 | 1964-03-02 | Process for the production of single crystal rods from silicon carbide |
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Citations (1)
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BE629139A (en) * | 1962-03-06 |
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