DE2149294C3 - Verfahren zur Härtung und zum Korrosionsschutz der Oberfläche eines Stahlstücks sowie Anwendung des bei Durchführung des Verfahrens erhaltenen Stahlstücks - Google Patents

Verfahren zur Härtung und zum Korrosionsschutz der Oberfläche eines Stahlstücks sowie Anwendung des bei Durchführung des Verfahrens erhaltenen Stahlstücks

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Publication number
DE2149294C3
DE2149294C3 DE2149294A DE2149294A DE2149294C3 DE 2149294 C3 DE2149294 C3 DE 2149294C3 DE 2149294 A DE2149294 A DE 2149294A DE 2149294 A DE2149294 A DE 2149294A DE 2149294 C3 DE2149294 C3 DE 2149294C3
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DE
Germany
Prior art keywords
layer
chromium
hardening
steel
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.)
Expired
Application number
DE2149294A
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English (en)
Other versions
DE2149294B2 (de
DE2149294A1 (de
Inventor
Werner Neuchatel Haenni
Hans E. Anet Bern Hintermann
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.)
Novartis AG
Original Assignee
Ciba Geigy AG
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Filing date
Publication date
Application filed by Ciba Geigy AG filed Critical Ciba Geigy AG
Publication of DE2149294A1 publication Critical patent/DE2149294A1/de
Publication of DE2149294B2 publication Critical patent/DE2149294B2/de
Application granted granted Critical
Publication of DE2149294C3 publication Critical patent/DE2149294C3/de
Expired legal-status Critical Current

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    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/36—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including layers graded in composition or physical properties
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C16/34—Nitrides
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C16/38—Borides
    • C—CHEMISTRY; METALLURGY
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    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C23C16/42—Silicides
    • C—CHEMISTRY; METALLURGY
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    • 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
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    • C—CHEMISTRY; METALLURGY
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    • Y10T428/12972—Containing 0.01-1.7% carbon [i.e., steel]

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Description

Für die Abscheidung des Chroms läßt man das so erhaltene Gemisch: Chromchlorid/Argon/Wasserstoff/ restliche Salzsäure sei es unmittelbar, sei es mit Wasserstoff verdünnt, auf den Grundwerkstoff einwirken. Man arbeitet unter atmosphärischem Druck mit großen Gasmengen oder selbst im Vakuum (vorzugsweise 50 bis 100 Torr), um so schnell wie möglich die gasförmigen Produkte zu entfernen, die normalerweise aus Salzsäure und Eisenchlorid bestehen.
Man kann die Zwischenschicht ebenfalls mit Hilfe mehrerer Metalle verwirklichen, z. B. eine erste Schicht aus Silizium und eine zweite aus Chrom niederschlagen.
Es empfiehlt sich darauf zu achter», daß die Zwischenschicht nicht weniger hart ist als der Grundwerkstoff.
Die härtende Endschicht, die an sich ebenso bekannt ist wie die für ihre Abscheidung verwendeten Mittel, wird ebenso auf chemischem Wege in der Gasphase erzeugt. Sie wird von einem Carbid, einem Nitrid, einem Silizid oder einem Borid eines temperaturfesten Metalls der Gruppen III bis VI des periodischen Systems gebildet, vorzugsweise vor. Nickelborid oder Tantal- oder Titancarbid. Beispielsweise im Falle des Titancarbids wird eine Titanverbindung, wie z. B. Titantetrachlorid, in einem Flüssigkeitsverdampfer verdampft und ständig dem Gasfluß zugefügt. Methan, Äthin oder Äthylen beispielsweise könnne direkt im gasförmigen Zustand eingeführt werden, Dicyclopentadien muß vorher in den dampfförmigen Zustand überführt werden.
Man läßt beispielsweise das gasförmige Gemisch CH4ITiCl4=H2 in den Verhältnissen 1:1:100 bis 5: 5:100 auf den Grundwerkstoff in einem Reaktor einwirken, dessen wesentliche Teile aus 80% Ni, 14% Cr, 6% Fe bestehen, indem man darauf achtet, daß alle Eisenteile vermieden werden,
ίο Nach der Gleichung
CH4 + TiIC4 —i- TiC + 4HCI (III)
sind die Produkte voluminöser, und deshalb arbeitet man in einem Vakuum von 10 bis 100 Torr (Temperatur von 800 bis 9000C).
Man kann die härtende Schicht ebenfalls in Form einer Aluminiumoxid-Schicht verwirklichen oder auch als kombinierte Schicht, z. B. aus Chromcarbid und Titancarbid oder aus Titancarbid und Titannitrid, um Farbnuancen zwischen silberfarbig und goldfarbig zu erhalten.
Das Verfahren nach der Erfindung gestattet, alle harten und korrosionsfesten Stücke herzustellen, insbesondere Teile von Uhrgehäusen, wie z. B. Gehäusemittelteile, Deckelringe, deren Abdeckungen usw.

Claims (2)

  1. Titancarbid besteht Im Falle des Chroms hat die
    Patentansprüche: Erfahrung gezeigt, daß das niedergeschlagene Metall
    mit dem Kohlenstoff des Stahls Chromcarbide bildet,
    1, Verfahren zur Härtung und zum Korrosions- die sich besonders gut als Carbidbasis bei dem abschutz der Oberfläche eines Stahlstücks durch Ab- 5 schließenden Niederschlag der härtenden Titancarbidscheidung einer härtenden Schicht auf einer auf Schicht eignen.
    dem Grundwerkstoff aufgetragenen Zwischen- Bei der Chromierung spielen sich die beiden nachschiebt, dadurch gekennzeichnet, daß stehenden Reaktionen ab, von denen entweder die man auf dem Stahlstück eine mindestens teilweise eine oder die andere überwiegt je nach der Art des in den Grundwerkstoff eindiffundierende Zwischen- io gewählten Reduktionsmittels, sei es Wasserstoff oder schicht aus mindestens einem der passivierbaren Metall:
    Metalle Chrom, Tantal, Aluminium, Silicium und CrCl8 + H2 -> Cr + 2HCl (I)
    Nickel aufbringt und darauf in bekannter Weise CrCl2 + Fe -> Cr + FeCl2 (II)
    auf chemischem Wege in der Gasphase eine
    härtende Schicht aus Titancarbid und/oder Titan- »5 Man geht aus von einem Chromhalogenid, z. B. nitrid, Chromcarbid, Tantalcarbid, Nickelborid von Chromtrichlorid, das in die Gleichungen 1 und II oder Aluminiumoxid abscheidet. der Einfachheit halber als CrCia eingeführt wird, das
  2. 2. Anwendung des Verfahrens nach Anspruch 1 aber in Wirklichkeit alle (11)- und (Ill)-Chromhalofür die Herstellung von harten und korrosions- genide in der Stufenfolge der Valenzen umfaßt. In festen Uhrengehäuseteilen. ao Gleichung I wird das Reduktionsmittel des Wasserstoffs allmählich dem Chromhalogenid zugefügt, während nach Gleichung II dies ein Metall ist, das
    gewöhnlich mit dem Grundwerkstoff, gegebenenfalls
    Eisen, übereinstimmt.
    25 Entsprechend den gewählten Parametern, Tem-
    Die Erfindung betrifft ein Verfahren zur Härtung peratur, Druck, Gaskonzentration, Grundwerkstoff und zum Korrosionsschutz der Oberfläche eines Stahl- usw. bildet sich an der Oberfläche der Probe eine vollstücks durch Abscheidung einer härtenden Schicht auf ständig oder teilweise diffundierte Chromschicht,
    einer auf dem Grundwerkstoff aufgetragenen Zwi- Die Niederschlagstemperaturen liegen vorzugsweise
    schenschicht. 30 oberhalb von 85O°C, damit ein ausreichend hoher
    Es sind Verfahren zur Herstellung von Überzügen Dampfdruck des Chromchlorids ausgeübt werden auf Eisenwerkstoffen bekannt, bei denen eine härtende kann.
    Schicht auf dem Werkstoff abgeschieden wird (DT-AS Fs lassen sich große Diffusionszonen in einem min-
    1142 261, 1092 271 und 1116 499). Es ist weiterhin destens 0,05% Kohlenstoff enthaltenden Stahl erbekannt, auf chemischem Weg in der Gasphase eine 35 zielen. Stähle, die ferritreich sind, und Stähle, die härtende Schicht abzuscheiden (DT-AS ί 069 448). Elemente enthalten, welche die Ferritphase bilden, Diese Verfahren sind jedoch nur für legierte oder oder Kohlenstoff-Stabilisatoren, wie z. B. Cr, Mo, W, nicht legierte Kohlenstoffstähle geeignet, so daß die V, Ta, Ti, Zr, Al, Si und Nb, begünstigen die Diffusk n. derart gehärteten Stücke anfällig für Korrosions- Wenn man von Wasserstoff auf Chromhalogenide
    angriffe sind. 40 als Zusatz übergeht, vermindert man die Reaktion des
    Der Erfindung liegt die Aufgabe zugrunde, unter Chromaustauschs (Gleichung II) und begünstigt die Vermeidung der vorgenannten Mängel ein Verfahren Niederschlags-Reakf'on (Gleichung I). Wenn man bereitzustellen, daß die gleichzeitige Härtung und den Kohlenstoffstahl' /C έ 0,2%), austenitischen Stahl Korrosionsschutz ermöglicht. oder Stähle benutzt, die Elemente enthalten, welche
    Diese Aufgabe wird erfindungsgemäß dadurch ge- 45 die austenitische Phase bilden, wie z. B. Ni, Mn, Cu löst, daß man auf dem Stahlstück eine mindestens teil- und N, vermindert man die Diffusion stark,
    weise in den Grundwerkstoff eindiffundierende Zwi- Beim Niederschlag des Chroms bilden die Stähle
    schenschicht aus mindestens einem der passivierbaren mit der Werkstoffnummer 1.2000 bis 1.3500 auf der Metalle Chrom, Tantal, Aluminium, Silicium und Oberfläche mit dem Kohlenstoff des Stahls Chrom-Nickel aufbringt und darauf in bekannter Weise auf 50 carbidschichten von guter Haftung, die porenfrei, hart chemischem Wege in der Gasphase eine härtende und verschleißfest sind.
    Schicht aus Titancarbid und/oder Titannitrid, Chrom- Man kann auch gasförmige Salzsäure auf metalli-
    carbid, Tantalcarbid, Nickelborid oder Aluminium- sches Chrom einwirken lassen, um CrCl2 zu bilden, oxid abscheidet. das anschließend zu metallischem Chrom in Schichtin Weiterausbildung der Erfindung erfolgt die An- 55 form reduziert wird. Man läßt ein Gemisch von Argon Wendung des Verfahrens für die Herstellung von harten und Salzsäure Ar: HCl 100:1 bis 20:1 bei Tem- und korrosionsfesten Uhrengehäuseteilen. peraturen ^ 90O0C (vorzugsweise 8500C) auf ge-
    Die mit der Erfindung erzielten Vorteile bestehen körntes oder pulverisiertes Chrom einwirken, das insbesondere darin, daß mit der als Überzug für Ver- gleichmäßig in einem ganz aus Aluminiumoxid beschleißteile vorgesehenen Doppelschicht eine ausge- 60 stehenden Behälter dispergiert ist; man nutzt also die zeichnete Korrosionsfestigkeit erzielt wird. Gleichgewichtsreaktion (Gleichung I) im entgegen-
    Bei einer bevorzugten Verwirklichung der Erfindung gesetzten Sinn aus.
    wird die aus mindestens einem passivierbaren Metall An Stelle der Salzsäure läßt sich elementares Chlor
    bestehende Zwischenschicht wie die härtende Schicht verwenden, um CrCl2 nach der folgenden Gleichung: in der Gasphase erzeugt. Das verwendete Metall 65 j
    kann Chrom, Tantal, Aluminium, Silizium, Nickel Cr -f Cla > CrCl2
    sein, wobei das letztere jedoch nur in Betracht kommt,
    wenn die abschließende, härtende Schicht nicht aus zu bilden.
DE2149294A 1970-10-02 1971-09-29 Verfahren zur Härtung und zum Korrosionsschutz der Oberfläche eines Stahlstücks sowie Anwendung des bei Durchführung des Verfahrens erhaltenen Stahlstücks Expired DE2149294C3 (de)

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JPS5165037A (ja) * 1974-12-03 1976-06-05 Seiko Instr & Electronics Tokeibuhin
IT1123082B (it) * 1975-11-14 1986-04-30 Fulmer Res Inst Ltd Matrice migliorata per dare forma a metallo,costituita da un substrato d'acciaio rivestito di uno strato contenente fosfuro di nichel,metodo per la sua preparazione e suo impiego per l'estrusione di alluminio
CH640885A5 (de) * 1978-07-21 1984-01-31 Suisse Horlogerie Rech Lab Mit einem harten ueberzug versehene maschinenelemente.
FR2451949A1 (fr) * 1979-03-22 1980-10-17 Nl Vintage Procede pour revetir des objets d'une surface en matiere dure que l'on puisse exploiter commercialement et objets fabriques par ce procede
US4278708A (en) * 1979-10-31 1981-07-14 Ford Motor Company Conductive corrosion resistant material and alkali metal/polysulfide battery employing same
CH643421B (fr) * 1980-04-10 Asu Composants Sa Procede de depot d'un revetement dur d'un compose d'or, cible de depot pour un tel procede et piece de joaillerie comportant un tel revetement.
DE3318999A1 (de) * 1983-05-25 1984-11-29 M.A.N. Maschinenfabrik Augsburg-Nürnberg AG, 8000 München Beschichteter metallischer gegenstand sowie verfahren zu dessen herstellung
US5514482A (en) * 1984-04-25 1996-05-07 Alliedsignal Inc. Thermal barrier coating system for superalloy components
EP0198078A4 (de) * 1984-10-17 1988-11-24 Stanford Res Inst Int Verfahren zum aufbringen von beschichtungen auf metalle und so hergestellte erzeugnisse.
EP0186266A1 (de) * 1984-11-19 1986-07-02 Avco Corporation Verschleissfestes Überzugssystem
EP0188057A1 (de) * 1984-11-19 1986-07-23 Avco Corporation Verschleissfeste Überzüge
FR2579997A1 (fr) * 1985-04-03 1986-10-10 Preci Coat Sa Procede de traitment de surface d'un objet et objet obtenu par ce procede
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US5217817A (en) * 1989-11-08 1993-06-08 U.S. Philips Corporation Steel tool provided with a boron layer
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DE59403689D1 (de) * 1993-03-16 1997-09-18 Balzers Hochvakuum Verfahren zur Standzeiterhöhung von Werkzeugen und Verschleissschutz-beschichtetes Werkzeug
JP3203256B2 (ja) * 1996-01-31 2001-08-27 日本板硝子株式会社 光モジュールおよびその製造方法
EP1237058A1 (de) * 2001-02-28 2002-09-04 Eta SA Fabriques d'Ebauches Benutzung einer nichtmagnetischen Schicht zum Abdecken von Teilen in einem Uhrengangwerk
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DE2149294B2 (de) 1975-02-20
JPS5474286A (en) 1979-06-14
CH1466870A4 (de) 1977-08-15
IT961073B (it) 1973-12-10
FR2110202A1 (de) 1972-06-02
IL37832A0 (en) 1971-12-29
GB1361427A (de) 1974-07-24
US3796588A (en) 1974-03-12
AT313018B (de) 1974-01-25
ES395606A1 (es) 1973-11-01
BR7106533D0 (pt) 1973-01-02
DE2149294A1 (de) 1972-04-06
FR2110202B1 (de) 1976-02-13
JPS5411779B1 (de) 1979-05-17
ZA716596B (en) 1972-08-30
NL7113545A (de) 1972-04-05
AU3412371A (en) 1973-04-05
CH600407B5 (de) 1978-06-15
CA956216A (en) 1974-10-15

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E77 Valid patent as to the heymanns-index 1977