DE1280019B - Crucible for the vapor deposition of aluminum layers under subatmospheric pressure - Google Patents

Crucible for the vapor deposition of aluminum layers under subatmospheric pressure

Info

Publication number
DE1280019B
DE1280019B DEU8209A DEU0008209A DE1280019B DE 1280019 B DE1280019 B DE 1280019B DE U8209 A DEU8209 A DE U8209A DE U0008209 A DEU0008209 A DE U0008209A DE 1280019 B DE1280019 B DE 1280019B
Authority
DE
Germany
Prior art keywords
crucible
vapor deposition
aluminum layers
subatmospheric pressure
layers under
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
Application number
DEU8209A
Other languages
German (de)
Inventor
Victor Mandorf Jun
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Union Carbide Corp
Original Assignee
Union Carbide Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Union Carbide Corp filed Critical Union Carbide Corp
Publication of DE1280019B publication Critical patent/DE1280019B/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/26Vacuum evaporation by resistance or inductive heating of the source
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/583Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride

Description

Tiegel zum Aufdampfen von Aluminiumschichten bei unteratmosphärischem Druck Aus der Auslegeschrift 1085 743 ist es bekannt, zum Verdampfen von Metallen, insbesondere von Aluminium, im Vakuum Tiegel aus geschmolzenen Boriden, insbesondere aus Zirkonborid, zu verwenden. Es ist ferner aus der Auslegeschrift D 19878 VI/48 b bekannt, Tiegel für diesen Zweck aus Boriden der Gruppe IVa/Va des Periodischen Systems herzustellen, die gegebenenfalls als Bindemittel noch Zusätze von Metallen, wie Kobalt oder Eisen, enthalten können. Obwohl diese Tiegel in mancher Beziehung gute Eigenschaften besitzen, so entsprechen sie doch nicht allen Anforderungen. Wegen der guten elektrischen Leitähigkeit der Boride ist eine große Strommenge erforderlich, um sie durch Widerstandsheizung auf die zum Verdampfen erforderliche Temperatur zu bringen. Das Aluminium verdampft aus solchen Tiegeln auch nicht immer mit der gewünschten Geschwindigkeit. Schließlich haben die bekannten Tiegel unter den Betriebsbedingungen eine nur beschränkte Lebensdauer.Crucible for the vapor deposition of aluminum layers in subatmospheric conditions Pressure From the Auslegeschrift 1085 743 it is known to evaporate metals, in particular of aluminum, in a vacuum crucible made of molten borides, in particular made of zirconium boride. It is also from the interpretation document D 19878 VI / 48 b known crucibles for this purpose made of borides of group IVa / Va of the periodic System that may contain additives of metals, such as cobalt or iron. Although these crucibles in some respects have good properties, they do not meet all requirements. Because of the good electrical conductivity of the borides, a large amount of electricity is required to bring them to the temperature required for evaporation by resistance heating bring to. The aluminum does not always evaporate from such crucibles with the desired speed. Finally, the known crucibles have under the operating conditions a limited lifespan.

Die Erfindung betrifft die Verwendung eines mittels eines hindurchgeleiteten elektrischen Stromes erhitzten Tiegels zum Aufdampfen von Aluminiumschichten, vorteilhaft bei einem hohen Vakuum. Diese Tiegel sind den bekannten Tiegeln in der oben beschriebenen Hinsicht überlegen.The invention relates to the use of a by means of a passed through Electric current heated crucible for the vapor deposition of aluminum layers, advantageous at a high vacuum. These crucibles are the known crucibles in the one described above Considerations.

Erfindungsgemäß bestehen diese Tiegel aus einem Gemisch von 30 bis 70 °/o Bornitrid und 70 bis 30 °/o eines elektrisch leitenden feuerfesten Materials, vorteilhaft Titandiborid. Tiegel nach der Erfindung zeichnen sich durch eine geringe elektrische Leitfähigkeit aus und können bequem durch Widerstands- oder Induktionsheizung auf die Verdarnpfungstemperatur des Metalls erhitzt werden. Sie werden von geschmolzenem Aluminium gut benetzt, ermöglichen eine hohe Verdampfungsgeschwindigkeit des Aluminiums und haben eine sehr lange Lebensdauer.According to the invention, these crucibles consist of a mixture of 30 to 70 ° / o boron nitride and 70 to 30 ° / o of an electrically conductive refractory material, advantageously titanium diboride. Crucibles according to the invention are characterized by a low electrical conductivity and can be comfortably achieved by resistance or induction heating heated to the evaporation temperature of the metal. You will be melted from Well-wetted aluminum enables a high rate of evaporation of the aluminum and have a very long lifespan.

Als elektrisch leitende feuerfeste Materialien kommen außer Titandiborid auch z. B. Zirkondiborid, Titancarbid oder Gemische dieser Stoffe in Betracht.Other electrically conductive refractory materials are titanium diboride also z. B. zirconium diboride, titanium carbide or mixtures of these substances into consideration.

Es ist zweckmäßig, zur Herstellung der Tiegel nach der Erfindung ein Bornitrid zu verwenden, das nicht mehr als 5 Gewichtsprozent Sauerstoff enthält. Geht man über diese Grenze hinaus, so kann bei hohen Betriebstemperaturen der Tiegel weich werden und seine Form verlieren.It is expedient to use one for the manufacture of the crucible according to the invention To use boron nitride, which contains no more than 5 percent by weight of oxygen. If you go beyond this limit, the crucible can become soft and lose its shape.

Zur Herstellung der beschriebenen Tiegel geht man so vor, daß man die Ausgangsstoffe in feinverteiltem Zustande mischt, formt und heiß preßt, wobei das Formen und das Pressen in einem Arbeitsgang durchgeführt werden können.To produce the crucible described, one proceeds in such a way that one mixes, molds and hot-presses the starting materials in a finely divided state, whereby the molding and the pressing can be carried out in one operation.

Die Ausgangsstoffe sollten vor dem Mischen fein zerkleinert werden, zweckmäßigerweise bis zum durchschnittlichenTeilchendurchmesser unter etwa 0,075mm. In der Regel empfiehlt es sich, Bornitrid mit einem durchschnittlichen Teilchendurchmesser von etwa 0,3 Mikron und die anderen Stoffe, z. B. Titandiborid, mit einem durchschnittlichen Teilchendurchmesser von etwa 15 oder 7 Mikron zu verarbeiten.The raw materials should be finely ground before mixing, suitably up to the average particle diameter below about 0.075 mm. Usually it is recommended to use boron nitride with an average particle diameter of about 0.3 microns and the other materials, e.g. B. titanium diboride, with an average Particle diameters of about 15 or 7 microns to be processed.

Das Formen und das Pressen werden bei hohen Temperaturen, z. B. bei 1700 bis 2000°C, und in der Regel unter Druck, z. B. von 35 bis 140 kg/cm2, durchgeführt.The molding and pressing are carried out at high temperatures, e.g. B. at 1700 to 2000 ° C, and usually under pressure, e.g. B. from 35 to 140 kg / cm2.

Die nachstehende Tabelle zeigt den spezifischen elektrischen Widerstand von Mischungen aus Titandiborid mit einer durchschnittlichen Teilchengröße von etwa 15 Mikron und Bornitrid mit einer durchschnittlichen Teilchengröße von 0,3 Mikron, die bei 1800°C und einem Druck von 140 kg/cmz verpreßt worden waren. Es sei bemerkt, daß diese Messungen bei 25°C durchgeführt worden sind. Die Mischungen haben einen positiven Temperaturkoeffizienten; bei 1400°C sind die spezifischen Widerstände etwa 21/9mal höher. Titandiborid Bomitrid spezifischer Gewichts- Volum- Gewichts- Volum- Widerstand in prozent prozent prozent prozent Mikron 70,0 I 53,8 30,0 46,2 180 59,0 41,8 41,0 58,2 900 55,0 37,8 45,0 ; 62,2 1560 53,0 36,0 47,0 64,0 2500 The table below shows the electrical resistivity of mixtures of titanium diboride with an average particle size of about 15 microns and boron nitride with an average particle size of 0.3 microns, which were pressed at 1800 ° C. and a pressure of 140 kg / cm 2. It should be noted that these measurements were made at 25 ° C. The mixtures have a positive temperature coefficient; at 1400 ° C the resistivities are about 21/9 times higher. Titanium diboride boron nitride more specific Weight- Volume- Weight- Volume- Resistance in percent percent percent percent microns 70.0 I 53.8 30.0 46.2 1 80 59.0 41.8 41.0 58.2 900 55.0 37.8 45.0; 62.2 1560 53.0 36.0 47.0 64.0 2500

Claims (1)

Patentanspruch: ; , Verwendung eines mittels elektrischer Widerstandsheizung erhitzbaren Tiegels aus einem Gemisch von 30 bis 70 °/o Bornitrid und 70 bis 30 °/o eines elektrisch leitenden feuerfesten Materials, vorzugsweise Titandiborid, zum Aufdampfen-von Aluminiumschichten bei unteratmosAärischerri Druck. In Betracht gezogene Druckschriften: Deutsche Auslegeschrift Nr. 1085-743; deutsche Auslegeschrift D 19&78 VI/48 b (bekanntgemacht am 17. 5.1956).Claim:; , Using a means of electrical resistance heating heatable crucible made of a mixture of 30 to 70% boron nitride and 70 to 30 ° / o of an electrically conductive refractory material, preferably titanium diboride, for the vapor deposition of aluminum layers with sub-atmospheric pressure. Into consideration Extracted publications: German Auslegeschrift No. 1085-743; German interpretation document D 19 & 78 VI / 48 b (published on May 17, 1956).
DEU8209A 1960-07-25 1961-07-22 Crucible for the vapor deposition of aluminum layers under subatmospheric pressure Pending DE1280019B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US1280019XA 1960-07-25 1960-07-25

Publications (1)

Publication Number Publication Date
DE1280019B true DE1280019B (en) 1968-10-10

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Family Applications (1)

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DEU8209A Pending DE1280019B (en) 1960-07-25 1961-07-22 Crucible for the vapor deposition of aluminum layers under subatmospheric pressure

Country Status (1)

Country Link
DE (1) DE1280019B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19955428A1 (en) * 1999-11-18 2001-06-07 Fraunhofer Ges Forschung Electron beam vaporizer, used for vaporizing aluminum, comprises high temperature container made of electrically-conducting ceramic for receiving vaporized material inserted into liquid-cooled crucible

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1085743B (en) * 1956-12-19 1960-07-21 Heraeus Gmbh W C Evaporation crucible made of electrically conductive chemical compounds

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1085743B (en) * 1956-12-19 1960-07-21 Heraeus Gmbh W C Evaporation crucible made of electrically conductive chemical compounds

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19955428A1 (en) * 1999-11-18 2001-06-07 Fraunhofer Ges Forschung Electron beam vaporizer, used for vaporizing aluminum, comprises high temperature container made of electrically-conducting ceramic for receiving vaporized material inserted into liquid-cooled crucible

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