DE4106745A1 - Plasma nitriding of aluminium@ (alloy) components - at temps. below component m.pt., producing very hard, wear- and corrosion-resistant aluminium nitride coatings - Google Patents

Plasma nitriding of aluminium@ (alloy) components - at temps. below component m.pt., producing very hard, wear- and corrosion-resistant aluminium nitride coatings

Info

Publication number
DE4106745A1
DE4106745A1 DE19914106745 DE4106745A DE4106745A1 DE 4106745 A1 DE4106745 A1 DE 4106745A1 DE 19914106745 DE19914106745 DE 19914106745 DE 4106745 A DE4106745 A DE 4106745A DE 4106745 A1 DE4106745 A1 DE 4106745A1
Authority
DE
Germany
Prior art keywords
plasma
nitriding
corrosion
wear
alloy
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.)
Withdrawn
Application number
DE19914106745
Other languages
German (de)
Inventor
Franz Prof Dr Katzer
Stephan Reichelt
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.)
KATZER, FRANZ, PROF. DR., 99099 ERFURT, DE
Original Assignee
PAEDAGOGISCHE HOCHSCHULE ERFUR
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 PAEDAGOGISCHE HOCHSCHULE ERFUR filed Critical PAEDAGOGISCHE HOCHSCHULE ERFUR
Priority to DE19914106745 priority Critical patent/DE4106745A1/en
Publication of DE4106745A1 publication Critical patent/DE4106745A1/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)

Abstract

Alumium (alloy) components undergo plasma nitriding, producing very hard, wear- and corrosion-resistant aluminium nitride protective coatings. The first stage involves cleaning of the component surface in an atmosphere of Ar, N2 or NH3, and subsequent removal of the natural oxide layer by sputtering. The second stage comprises nitriding of the aluminium, (or alloy) component in nitriding media (NH3, NH3/N2, NH3/H2 or N2/H2) by N2 in the form of a plasma. Plasma temperature is 350 deg.C-50 K below the m.pt. of the component material (or its lowest m.pt. grain-boundary impurities). Plasma nitriding is performed in conventional plasma nitriding equipment. USE/ADVANTAGE - Surface-coating of components used in pneumatic and hydraulic systems. Durability of the aluminium nitride coating is several times greater than that of eloxation coating

Description

Die Erfindung betrifft ein Verfahren zur Herstellung von Oberflächenschutzschichten auf Aluminiumbauteilen, insbesondere von solchen Bauteilen, die in der Fluidtechnik zur An­ wendung gelangen. Die Bauteile in der Fluidtechnik unter­ liegen einem intensiven Verschleiß- und Korrosionsregime, deshalb benötigen sie eine harte, verschleißfeste und kor­ rosionsstabile Oberfläche. Bisher wurden diese Aluminium­ bauteile mit ANOX- oder ANOF-Verfahren oberflächenveredelt. Mit den genannten Verfahren verschiebt sich die Korrosions­ stromdichte und das Ruhepotential zu positiven Werten, d. h. zu edlerem Verhalten hin. Verglichen mit adäquaten Schutz­ schichten auf Eisenwerkstoffen besitzen die verstärkten Oxidschichten auf Aluminiumwerkstoffen im Tribosystem unter vergleichbaren Beanspruchungsbedingungen eine geringere Le­ bensdauer. Bei Eisenwerkstoffen kann durch Einbringen von Stickstoff in die Oberflächenschichten (Nitrieren, Plasma nitrieren) eine harte, verschleißfeste und korrosionsstabile Schicht aufgebaut werden. Auch bei Aluminiumwerkstoffen ist durch Einbringen von Stickstoff in die Oberfläche und in oberflächennahe Schichten eine harte und verschleißfeste Schicht aufbaubar. Jedoch ist eine problemlose Übertragung der für Eisenwerkstoffe bewährten Nitrier- und Plasmani­ trierverfahren auf Aluminiumwerkstoffe nicht möglich.The invention relates to a method for producing Surface protective layers on aluminum components, in particular of such components that are used in fluid technology turn. The components in fluid technology under are subject to an intensive wear and corrosion regime, therefore you need a hard, wear-resistant and cor corrosion-resistant surface. So far, these were aluminum Components with ANOX or ANOF processes are surface-finished. With the methods mentioned, the corrosion shifts current density and the resting potential to positive values, d. H. towards more noble behavior. Compared to adequate protection layers on ferrous materials have the reinforced Oxide layers on aluminum materials in the tribological system below comparable stress conditions a lower Le lifetime. In the case of ferrous materials, the introduction of Nitrogen in the surface layers (nitriding, plasma nitriding) a hard, wear-resistant and corrosion-resistant Layer. Even with aluminum materials is by introducing nitrogen into the surface and a hard and wear-resistant layer close to the surface Buildable layer. However, transmission is problem-free the nitriding and plasmani proven for iron materials Not possible to process on aluminum materials.

Bekannt ist das Nitrieren von Aluminiumpulver (nach EP 0158-271) zum Gewinnen von Aluminiumnitridpulver (AlN). Dieses Verfahren und die anderen bekannten Verfahren zur Herstellung von AlN-Pulver können nicht für die Nitrierung von Bauteilen angewendet werden, da sie den metallischen Grund­ stoff in Pulverform voraussetzen oder bei Temperaturen ablaufen, die oberhalb der Schmelztemperatur von Aluminium liegen.The nitriding of aluminum powder is known (according to EP 0158-271) for the extraction of aluminum nitride powder (AlN). This Methods and the other known methods of manufacture of AlN powder cannot be used for nitriding Components are applied as they cover the metallic background  Require powder material or at temperatures expire above the melting temperature of aluminum lie.

Die Erfindung verfolgt daher das Ziel fertigge­ formte Bauteile aus Aluminiumwerkstoffen mit einer stabilen, fest dem Grundwerkstoff verbundenen, korrosions- und verschleißfesten Schutzschicht aus Aluminiumnitrid zu ver­ sehen. Das Verfahren soll auf der Plasmatechnologie basieren und mit herkömmlichen Plasmanitrieranlagen ohne Umbau und ohne zusätzliche Einrichtung ausführbar sein.The invention therefore pursues the goal finish molded components made of aluminum materials with a stable, firmly attached to the base material, corrosion and wear-resistant protective layer made of aluminum nitride see. The process is to be based on plasma technology and with conventional plasma nitriding systems without modification and be executable without additional equipment.

Erfindungsgemäß wird die Aufgabe dadurch gelöst, indem in einer ersten Phase die Bauteiloberfläche, wie auch bei Eisen­ werkstoffen üblich, endgültig in einer Argon-, Stick­ stoff- oder Ammoniakatmosphäre gereinigt und anschließend durch Sputtern die natürliche Oxidschicht vollständig ent­ fernt wird. In der darauffolgenden 2. Phase erfolgt die eigentliche Nitrierung, indem Stickstoff, der durch Plasma bereitgestellt wird, in die Bauteiloberfläche eindringt bzw. durch chemische Reaktionen eine Aluminiumnitridschicht bildet, wobei die Plasmatemperatur im Bereich von 350°C bis 50 K unter der Schmelztemperatur des Werkstoffs bzw. seiner niedrigschmelzenden Korngrenzenverunreinigungen liegt (vgl. Zustandsschaubild). Als Nitriermedien kommen in Frage:According to the invention the object is achieved in that a first phase, the component surface, as with iron usual materials, finally in an argon, stick Cloth or ammonia atmosphere cleaned and then by sputtering completely remove the natural oxide layer is removed. In the subsequent 2nd phase the actual nitriding by adding nitrogen by plasma is provided, penetrates into the component surface or an aluminum nitride layer through chemical reactions forms, the plasma temperature in the range of 350 ° C. up to 50 K below the melting temperature of the material or its low melting grain boundary impurities lies (see state diagram). Come as nitrating media in question:

  • 1. Ammoniak1. ammonia
  • 2. Ammoniak-Stickstoff-Gemische2. Ammonia-nitrogen mixtures
  • 3. Ammoniak-Wasserstoff-Gemische3. Ammonia-hydrogen mixtures
  • 4. Stickstoff-Wasserstoff-Gemische4. Nitrogen-hydrogen mixtures

Die so erzeugte Aluminiumnitridschicht ist sehr hart, kor­ rosions- und verschleißfest, chemisch resistent gegen Nicht­ eisen-Metallschmelzen und thermoschockbeständig. Ihre Halt­ barkeit übertrifft die von eloxierten Schichten um ein mehr­ faches. Der spezifische elektrische Widerstand beträgt 20 · 10¹¹ Ohm · cm bei 25°C, was sich positiv auf die Kor­ rosionsfestigkeit auswirkt. Die Wärmeleitfähigkeit beträgt 180 W · m-1 · K-1, was der Gefahr des Abplatzens der Schicht durch Thermospannungen entgegenwirkt. Nach der Behandlung besitzen die Bauteile durch die Aluminiumnitridschicht ein dunkelgraues Aussehen. Die Dicke der Nitrierschicht sollte günstigerweise etwa 20 . . . 25 µm betragen, die sich etwa nach einer 4stündigen Behandlung eingestellt hat.The aluminum nitride layer produced in this way is very hard, corrosion and wear-resistant, chemically resistant to non-ferrous metal melts and resistant to thermal shock. Their durability exceeds that of anodized layers by a multiple. The specific electrical resistance is 20 · 10¹¹ Ohm · cm at 25 ° C, which has a positive effect on the corrosion resistance. The thermal conductivity is 180 W · m -1 · K -1 , which counteracts the risk of the layer flaking off due to thermal stresses. After the treatment, the components have a dark gray appearance due to the aluminum nitride layer. The thickness of the nitriding layer should conveniently be about 20. . . Amount to 25 µm, which has set in after a 4-hour treatment.

Die im folgenden aufgeführten Werte der Prozeßstufen ergeben bereits eine Schichtdicke von ca. 20 µm.The values of the process stages listed below result already a layer thickness of approx. 20 µm.

Claims (1)

Verfahren zur Herstellung von Aluminiumnitridschichten auf Bauteilen aus Aluminium bzw. aus Aluminiumlegierungen zur Erzeugung harter, verschleiß- und korrosionsfester Schutzschichten auf der Basis des Plasmanitrierens wobei nach einer in der 1. Phase erfolgten Reinigung der Bau­ teiloberfläche und einem restlosen Entfernen der natürlichen Oxidschicht durch Sputtern in der 2. Phase die eigentliche Nitrierung in bekannten Nitriermedien stattfindet, wobei der Stickstoff als Plasma zur Verfügung gestellt wird, dadurch gekennzeichnet, daß
  • - die Plasmatemperatur im Bereich von 350°C bis 50 K unter der Schmelztemperatur des Werkstoffs bzw. seiner nie­ drigschmelzenden Korngrenzenverunreinigungen liegt und daß
  • - die Plasmanitrierung in herkömmlichen Plasmanitrieranlagen ausgeführt werden kann.
Process for the production of aluminum nitride layers on components made of aluminum or of aluminum alloys for the production of hard, wear-resistant and corrosion-resistant protective layers based on plasma nitriding the 2nd phase the actual nitration takes place in known nitration media, the nitrogen being made available as plasma, characterized in that
  • - The plasma temperature is in the range of 350 ° C to 50 K below the melting temperature of the material or its never-melting grain boundary impurities and that
  • - The plasma nitriding can be carried out in conventional plasma nitriding systems.
DE19914106745 1991-03-02 1991-03-02 Plasma nitriding of aluminium@ (alloy) components - at temps. below component m.pt., producing very hard, wear- and corrosion-resistant aluminium nitride coatings Withdrawn DE4106745A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE19914106745 DE4106745A1 (en) 1991-03-02 1991-03-02 Plasma nitriding of aluminium@ (alloy) components - at temps. below component m.pt., producing very hard, wear- and corrosion-resistant aluminium nitride coatings

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19914106745 DE4106745A1 (en) 1991-03-02 1991-03-02 Plasma nitriding of aluminium@ (alloy) components - at temps. below component m.pt., producing very hard, wear- and corrosion-resistant aluminium nitride coatings

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DE4106745A1 true DE4106745A1 (en) 1992-09-03

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0666334A1 (en) * 1993-10-05 1995-08-09 Toyota Jidosha Kabushiki Kaisha Case nitrided aluminum product, process for case nitriding the same, and nitriding agent for the same
DE19519535A1 (en) * 1995-05-27 1996-11-28 Audi Ag Process for machining the surfaces of workpieces
GB2324539A (en) * 1997-04-26 1998-10-28 Daimler Benz Ag Aluminium nitride coating of cylinder running surface
US5888269A (en) * 1993-10-05 1999-03-30 Toyota Jidosha Kabushiki Kaisha Nitriding agent
EP1591551A1 (en) * 2003-01-24 2005-11-02 Research Institute for Applied Sciences ALUMINUM MATERIAL HAVING AlN REGION ON THE SURFACE THEREOF AND METHOD FOR PRODUCTION THEREOF
CN110670013A (en) * 2019-10-14 2020-01-10 中信戴卡股份有限公司 Surface treatment method of aluminum alloy hub and aluminum alloy hub

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5888269A (en) * 1993-10-05 1999-03-30 Toyota Jidosha Kabushiki Kaisha Nitriding agent
US5514225A (en) * 1993-10-05 1996-05-07 Toyota Jidosha Kabushiki Kaisha Case nitrided aluminum product, process for case nitriding the same, and nitriding agent for the same
US5582655A (en) * 1993-10-05 1996-12-10 Toyota Jidosha Kabushiki Kaisha Case nitrided aluminum product, process for case nitriding the same, and nitriding agent for the same
EP0666334A1 (en) * 1993-10-05 1995-08-09 Toyota Jidosha Kabushiki Kaisha Case nitrided aluminum product, process for case nitriding the same, and nitriding agent for the same
DE19519535A1 (en) * 1995-05-27 1996-11-28 Audi Ag Process for machining the surfaces of workpieces
GB2324539A (en) * 1997-04-26 1998-10-28 Daimler Benz Ag Aluminium nitride coating of cylinder running surface
FR2762618A1 (en) * 1997-04-26 1998-10-30 Daimler Benz Ag PROCESS FOR COATING ALUMINUM NITRIDE OF THE CYLINDER PUT OF AN ALUMINUM ALLOY CASING
GB2324539B (en) * 1997-04-26 2000-01-26 Daimler Benz Ag Method for aluminium nitride coating
US6180189B1 (en) 1997-04-26 2001-01-30 Daimlerchrysler Ag Method and apparatus for aluminum nitride coating of a contact surface, especially a cylinder contact surface of a crankcase made of an aluminum basic alloy
DE19717825B4 (en) * 1997-04-26 2004-03-04 Daimlerchrysler Ag Process for aluminum nitride coating of the cylinder surface of a crankcase made of an Al-based alloy and corresponding crankcase
EP1591551A1 (en) * 2003-01-24 2005-11-02 Research Institute for Applied Sciences ALUMINUM MATERIAL HAVING AlN REGION ON THE SURFACE THEREOF AND METHOD FOR PRODUCTION THEREOF
EP1591551A4 (en) * 2003-01-24 2008-04-16 Res Inst For Applied Sciences ALUMINUM MATERIAL HAVING AlN REGION ON THE SURFACE THEREOF AND METHOD FOR PRODUCTION THEREOF
CN110670013A (en) * 2019-10-14 2020-01-10 中信戴卡股份有限公司 Surface treatment method of aluminum alloy hub and aluminum alloy hub

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Legal Events

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8139 Disposal/non-payment of the annual fee
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8170 Reinstatement of the former position
8127 New person/name/address of the applicant

Owner name: KATZER, FRANZ, PROF. DR., 99099 ERFURT, DE

8141 Disposal/no request for examination
8110 Request for examination paragraph 44
8170 Reinstatement of the former position
8139 Disposal/non-payment of the annual fee