DE2131407A1 - Gas depositon of dense silicon layers - on graphite bodies and fibres - Google Patents
Gas depositon of dense silicon layers - on graphite bodies and fibresInfo
- Publication number
- DE2131407A1 DE2131407A1 DE19712131407 DE2131407A DE2131407A1 DE 2131407 A1 DE2131407 A1 DE 2131407A1 DE 19712131407 DE19712131407 DE 19712131407 DE 2131407 A DE2131407 A DE 2131407A DE 2131407 A1 DE2131407 A1 DE 2131407A1
- Authority
- DE
- Germany
- Prior art keywords
- layer
- silicon
- gas
- pyrographite
- silicon carbide
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
- C04B41/5059—Silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
Verfahren zur Gasabscheidung dichter Siliziumkarbid-Schichten Die Erfindung bezieht sich auf ein Verfahren zur Gasabscheidung dichter Siliziumkarbid-Schichten, vorzugsweise zum Oxydationsschutz von Graphitkörpern und Graphitfasern.Process for the gas deposition of dense silicon carbide layers The invention relates to a method for gas deposition of dense silicon carbide layers, preferably for protection against oxidation of graphite bodies and graphite fibers.
Bekannt ist die Abscheidung von Siliziumkarbid-Schichten aus einer Gasphase auf Graphitkörpern oder sogenannten Refractory-Metallen durch Reduktion von silizium- und graphithaltigen Verbindungen, wie beispielsweise CII SiCl zum Schutz des Trägers 3 3 gegen Oxidation. IIierbei wächst auf dem erhitzten Trägermaterial (Substrat) eine mehr oder weniger dichte Siliziukarbid-Schicht auf, die je nach dem Ausdehnungskoeffizienten des Trägers mehr oder weniger stark haftet. Um nun den unter der Schicht liegenden Träger wirklich gut vor Oxidation zu schützen, müssen relativ dlcke Schichten von 10 - 100 ( Stärke abgeschieden werden. Diese dicken Schichten sind jedoch gegenüber Rißbildungen, vorallem bei Abweichung der Ausdehnungskoeffizienten zwischen Träger und Schicht, besonders empfindlich.The deposition of silicon carbide layers from one is known Gas phase on graphite bodies or so-called refractory metals through reduction of silicon and graphite-containing compounds, such as CII SiCl for Protection of the carrier 3 3 against oxidation. This grows on the heated substrate (Substrate) a more or less dense silicon carbide layer, depending on the adheres to the expansion coefficient of the carrier more or less strongly. To now to protect the carrier lying under the layer really well against oxidation relatively thick layers of 10 - 100 (thickness can be deposited. These thick Layers are, however, against the formation of cracks, especially in the event of a deviation in the expansion coefficient between carrier and layer, particularly sensitive.
Der vorliegenden Erfindung liegt die Aufgabe zugrunde, ein Verfahren zur Gasphasenabscheidung dünner, jedoch sehr dichter Siliziumkarbid-Schichten aufzuzeigen, bei dem äußerst dünne Schichten auf ein Tragermaterial aufgebracht werden können, die wegen ihrer geringen Dicke weniger rißempfindlich sind und die auch bei hohen Temperaturen das darunterliegende EIaterial vor Oxidation schützen.The present invention is based on the object of a method for the vapor deposition of thin, but very dense silicon carbide layers, in which extremely thin layers can be applied to a carrier material, which are less susceptible to cracking because of their small thickness and which are also high Temperatures protect the underlying egg material from oxidation.
Diese Aufgabe wird dadurch gelöst, daß zunächst auf dem bis ca 10000 C erhitzten Substrat in an sich bekannter Weise eine 1 bis 10 - dicke, sehr dichte Py.rographitschicht abgeschieden wird und in einem anschließenden Verfahrensschritt Substrat mit Pyrographit-Schicht auf eine Temperatur von etwas über 14200 C gebracht und der Reaktion einer siliziumhaltigen Verbindung und Wasserstoff - beispielsweise mit Wasserstoff verdünntem SiIIC13, SiC14 oder Sill4 - ausgesetzt wird. Hierdurch wird die Pyrographit-Schicht in eine Siliziumkarbid-Schicht umgewandelt.This object is achieved in that first on the to about 10,000 C, a 1 to 10-thick, very dense substrate is heated in a manner known per se Py.rographitschicht is deposited and in a subsequent process step Substrate with Pyrographite layer to a temperature slightly above 14200 C and the reaction of a silicon-containing compound and hydrogen - for example SiIIC13, SiC14 or Sill4 diluted with hydrogen - exposed will. This converts the pyrographite layer into a silicon carbide layer.
Der Vorteil dieser Maßnahmen ist darin zu sehen, daß die gewonnene Schutzschicht eine große Haftfähigkeit und eine absolute Gasdichtigkeit aufweist. Bei der Aufbringung einer derartigen Siliziumkarbid-Schicht auf Graphitfäden wird deren Diegsamkeit nicht wesentlich beeinträchtigt und bei Einbettung dieser den in anderen Materialien wird die Legierungsbildung verhindert.The advantage of these measures is to be seen in the fact that the Protective layer has great adhesiveness and absolute gas tightness. When applying such a silicon carbide layer to graphite threads whose looseness is not significantly impaired and when these are embedded the the formation of alloys is prevented in other materials.
Die Erfindung ist nachfolgend an einem Ausführungsbeispiel bes ciiri eben.The invention is described below using an exemplary embodiment just.
In einem Ofen 20 wird ein Substrat 10 gemäß dem Aúsführungsoeispiel ein Graphitkörper aus Elektrographit oder eine Graphitfaser - einer Temperatur von ca. 1000° C ausgesetzt und so in bekannter Weise mit einer 1 - 10 starken Pyrographit-Schicht 11 allseitig versehen. Diese Schicht ist vollkommen gasdicht.In a furnace 20, a substrate 10 according to the embodiment a graphite body made of electrographite or a graphite fiber - a temperature of exposed to approx. 1000 ° C and thus in a known manner with a 1 - 10 thick pyrographite layer 11 provided on all sides. This layer is completely gas-tight.
In dem nächsten Verfahrensschritt wird das Substrat auf eine Temperatur erbracht, die kurz über dem Schmelzpunkt von Silizium liegt, also etwas über 14200 C. Ist diese Temperatur erreicht, so wird das Gemisch 12 einer siliziumhaltigen Verbindung und wasserstoff - beispielsweise SiItC13, SiC14 oder SiH4 mit Wasserstoff verdünnt - in den Reaktionsraum geleitet. Auf der heißen Substratoberfläche findet die Reduktion der siliziumhaltigen Xrorbindung durch den Wasserstoff statt. Das hierbei ent5tehende Silizium ist bei der herrschenden Substrattemperatur schmelzflüssig und reagiert mit der Pyrographitschicht zu Silizium-Karbid Die dabei auf dem Substrat entstehende Siliziumkarbid-Schicht 1 ist durch die Menge der vorgegebenen Pyrographit-Schicht bestimmt. Nach Verbrauch dieser letztgenannten Schicht entsprechend obiger Reaktionsgleichung wird etwaiges später abgeschiedenes Silizium als polikristalline Siliziun-Schicht aufwachsen. Diese Schicht kann später sehr leicht durch Ätzbehandlung in einem Salpeter-Flußsäuregemi Sch abgetragen werden.In the next process step, the substrate is brought to a temperature that is just above the melting point of silicon, i.e. slightly above 14200 C. When this temperature is reached, the mixture 12 is a silicon-containing compound and hydrogen - for example SiItC13, SiC14 or SiH4 Diluted hydrogen - passed into the reaction chamber. On the hot substrate surface the reduction of the silicon-containing xorbond by the hydrogen takes place. The resulting silicon is molten at the prevailing substrate temperature and reacts with the pyrographite layer to form silicon carbide The silicon carbide layer 1 formed on the substrate is determined by the amount of the specified pyrographite layer. After this last-mentioned layer has been consumed in accordance with the above reaction equation, any silicon deposited later will grow as a polycrystalline silicon layer. This layer can later be removed very easily by etching in a nitric-hydrofluoric acid mixture.
Die entstehende SiC-Schicht 11 ist außerordentlich feinkörnig und dicht und daher besonders osydations s chütz end . Lin speziel -les Merkmal dieses Verfahrens ist, daß das Silizium nur mit der iyrographit-Schicht reagiert und wegen deren großer Dichte nIcht in den darunterliegenden Substratkörpey eindringen kann. Dies hat den Vorteil, daß im Inneren des Substratkörpers selbst keine Siliziumkarbid-Bildung erfolgen kann und damit auch eine mögliche Sprengung des Substratkörpers vermieden wird. Ein weiterer Vorteil ist, daß als Gasgemisch nur eine siliziumhaltige Verbindung erforderlich ist, da der Kohlenstoff zur Bildung des SiC aus der Pyrographitschicht entnommen wird.The resulting SiC layer 11 is extremely fine-grained and dense and therefore particularly protective against oxidation. Lin special feature of this Process is that the silicon only reacts with the iyrographite layer and because of whose high density cannot penetrate into the underlying substrate body. This has the advantage that there is no silicon carbide formation inside the substrate body itself can take place and thus also avoids a possible explosion of the substrate body will. Another advantage is that only a silicon-containing compound is used as the gas mixture is required because the carbon is used to form the SiC from the pyrographite layer is removed.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19712131407 DE2131407C3 (en) | 1971-06-24 | 1971-06-24 | Process for the gas deposition of a dense silicon carbide layer |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19712131407 DE2131407C3 (en) | 1971-06-24 | 1971-06-24 | Process for the gas deposition of a dense silicon carbide layer |
Publications (3)
Publication Number | Publication Date |
---|---|
DE2131407A1 true DE2131407A1 (en) | 1973-01-11 |
DE2131407B2 DE2131407B2 (en) | 1980-12-11 |
DE2131407C3 DE2131407C3 (en) | 1981-12-10 |
Family
ID=5811707
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19712131407 Expired DE2131407C3 (en) | 1971-06-24 | 1971-06-24 | Process for the gas deposition of a dense silicon carbide layer |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE2131407C3 (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2567120A1 (en) * | 1984-07-05 | 1986-01-10 | United Technologies Corp | Composite SiC/Si3N4 coatings or carbon-carbon composite materials |
US4702960A (en) * | 1980-07-30 | 1987-10-27 | Avco Corporation | Surface treatment for carbon and product |
US4752503A (en) * | 1984-07-20 | 1988-06-21 | Societe Europeenne De Propulsion | Process for the manufacture of a composite material with refractory fibrous reinforcement and ceramic matrix |
US4871587A (en) * | 1982-06-22 | 1989-10-03 | Harry Levin | Process for coating an object with silicon carbide |
US4921725A (en) * | 1986-12-04 | 1990-05-01 | Centre National De La Recherche Scientifique (Cnrs) | Process for coating carbon fibers with a carbide |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3372671A (en) * | 1965-05-26 | 1968-03-12 | Westinghouse Electric Corp | Apparatus for producing vapor growth of silicon crystals |
-
1971
- 1971-06-24 DE DE19712131407 patent/DE2131407C3/en not_active Expired
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3372671A (en) * | 1965-05-26 | 1968-03-12 | Westinghouse Electric Corp | Apparatus for producing vapor growth of silicon crystals |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4702960A (en) * | 1980-07-30 | 1987-10-27 | Avco Corporation | Surface treatment for carbon and product |
US4871587A (en) * | 1982-06-22 | 1989-10-03 | Harry Levin | Process for coating an object with silicon carbide |
FR2567120A1 (en) * | 1984-07-05 | 1986-01-10 | United Technologies Corp | Composite SiC/Si3N4 coatings or carbon-carbon composite materials |
US4752503A (en) * | 1984-07-20 | 1988-06-21 | Societe Europeenne De Propulsion | Process for the manufacture of a composite material with refractory fibrous reinforcement and ceramic matrix |
US5026604A (en) * | 1984-07-20 | 1991-06-25 | Societe Europeenne De Propulsion | Composite material with refractory fibrous reinforcement and ceramic matrix |
US4921725A (en) * | 1986-12-04 | 1990-05-01 | Centre National De La Recherche Scientifique (Cnrs) | Process for coating carbon fibers with a carbide |
Also Published As
Publication number | Publication date |
---|---|
DE2131407C3 (en) | 1981-12-10 |
DE2131407B2 (en) | 1980-12-11 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
OGA | New person/name/address of the applicant | ||
8326 | Change of the secondary classification | ||
C3 | Grant after two publication steps (3rd publication) | ||
8339 | Ceased/non-payment of the annual fee |