WO1999014393A1 - PROCEDE POUR REVETIR DES SUBSTRATS AVEC DE L'OXYDE D'ALUMINIUM (Al2O3) ET PIECE REVETUE SELON CE PROCEDE - Google Patents

PROCEDE POUR REVETIR DES SUBSTRATS AVEC DE L'OXYDE D'ALUMINIUM (Al2O3) ET PIECE REVETUE SELON CE PROCEDE Download PDF

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Publication number
WO1999014393A1
WO1999014393A1 PCT/EP1998/005909 EP9805909W WO9914393A1 WO 1999014393 A1 WO1999014393 A1 WO 1999014393A1 EP 9805909 W EP9805909 W EP 9805909W WO 9914393 A1 WO9914393 A1 WO 9914393A1
Authority
WO
WIPO (PCT)
Prior art keywords
coating
substrates
aluminum oxide
substrate
hollow cathode
Prior art date
Application number
PCT/EP1998/005909
Other languages
German (de)
English (en)
Inventor
Thomas LÖHKEN
Holger Lüthje
Cornelia Steinberg
Thomas Jung
Original Assignee
Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
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
Priority claimed from DE19830206A external-priority patent/DE19830206C2/de
Application filed by Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V.
Priority to EP98951423A priority Critical patent/EP1015654A1/fr
Publication of WO1999014393A1 publication Critical patent/WO1999014393A1/fr

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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium

Definitions

  • the invention relates to a method for coating substrates with aluminum oxide (Al 2 O 3 ) with at least a proportion of the crystalline phase of the aluminum oxide.
  • the invention further relates to a workpiece coated with this method.
  • Layers of aluminum oxide are characterized by great hardness, very good electrical insulation and high wear resistance. For these reasons, aluminum oxide coatings are applied for a wide variety of applications.
  • alpha modification of the aluminum oxide, ie the crystalline phase of the aluminum oxide, offers particular advantages, in particular when coating tools. However, this phase can only be achieved under special conditions. If coating with low temperatures, only one coating is used achieved with amorphous aluminum oxide or with the gamma modification, as is proposed, for example, in DE 196 12 344 C1 for coating plastic films.
  • the gas phase deposition method has proven particularly suitable and suitable for coating with at least a proportion of crystalline phase of the aluminum oxide. It is widely used and usually works at temperatures above 1,000 ° C, such as Prengel et al., CVD coatings based on medium temperature CVD Gamma- and ⁇ -AI 2 O 3 , in: Surface and Coatings Techn. 68 / 69 (1994) 217-220. At these high, usually still higher temperatures, this method enables a very good and mature coating of high quality and also cost-effective procedure.
  • CVD chemical vapor deposition
  • EP 0 513 662 B1 proposes the use of chromium as an auxiliary in the deposition, as a result of which a hard layer with (Al, Cr) 2 O 3 is to be formed, which are also coated with temperatures of around 900 ° C. by means of the CVD process can.
  • the use of the auxiliary chromium does not, of course, result in an aluminum oxide layer, as is actually desired, and the deposition rates are also quite low.
  • the object of the invention is a high-quality coating with aluminum oxide with at least partial ⁇ -crystalline phase To provide that can be done at relatively low temperatures and is still economical.
  • the substrates are coated by means of hollow cathode gas sputtering at temperatures of more than 400 ° C. and less than 1,000 ° C.
  • Hollow cathode gas flow sputtering is a well-known and proven method for high-rate coating with amorphous layers at low substrate temperatures.
  • the resulting layers which are known from the prior art, are all X-ray amorphous and, with a hardness of 1,400, measured by the Knoop method at a load of 0.025 pond, are significantly softer than the layers of crystalline ⁇ - Alumina.
  • Hollow cathode gas flow sputtering is significantly less expensive than pulse sputtering, which creates a much more economical coating option.
  • the hollow cathode gas flow sputtering preferably takes place at temperatures below 900 ° C., particularly preferably below 600 ° C. This means that tool steels, insulators and glasses can be coated economically and effectively with the hollow cathode gas flow sputter.
  • the deposition rates found in tests could be achieved up to over 50 ⁇ m / h, sometimes up to 100 ⁇ m / h.
  • the quality of the coating obtained is such that dielectrics, but also wear protection layers and friction-reducing layers can be achieved.
  • the coating process is preferably carried out at pressures between 0.1 and 10 hPa. It is particularly preferred if just enough oxygen (O 2 ) is added that the target of the hollow cathode is not yet oxidized. This oxygen number can be set properly, since the beginning oxidation of the target can immediately be measured in a change in the target properties. This setting enables stoichiometric Al 2 O 3 layers to be generated.
  • the targets present there are driven reactively, that is by means of alternating current.
  • the oxide formation takes place there on the target, and the oxidized aluminum oxide particles are transferred to the substrate as a whole.
  • the oxide formation only takes place on the substrate itself.
  • the oxygen content is preferably approximately 0.5 to 2%, in particular approximately 1% of the argon content.
  • argon another noble gas can also be used, the proportions then being able to be distributed differently.
  • graded layer systems according to the invention can be achieved, that is to say those in which the layer properties differ within the aluminum oxide. In this way, a somewhat softer and more elastic layer can be applied, which then changes into a harder aluminum oxide layer during further coating. This can be achieved simply by adjusting and varying the amount of O 2 supplied. If necessary, aluminum oxide with ⁇ phase would form and form parts of the layer.
  • the properties of the hollow cathode gas flow sputtering have a particularly favorable effect, since the gas stream flowing onto the substrate reaches the tips or small components unhindered, without backflow forming on a flat area, which could hinder the deposition process.
  • the substrates are moved in front of the hollow cathode.
  • the substrates are moved in front of the hollow cathode.
  • An alternative possibility, or one that can also be used simultaneously, is to provide two or more parallel gas flow hollow cathode sputtering sources in the same space, which also facilitates the coating of the layer systems with their gradations.
  • the substrates are connected to a voltage source.
  • a DC voltage source with a positive bias voltage and a potential between 10 volts and 1,000 volts is preferred.
  • Figure 1 is a schematic representation of a hollow cathode arrangement for performing the method
  • Figure 2 is a schematic representation of a coated substrate.
  • a substrate 10 is a flat disk here.
  • other bodies can also be involved, in particular tips and / or cutting edges which are to be coated are suitable.
  • the substrate is brought from the rear to a desired temperature via a substrate heater 12, here for example 600 ° C.
  • the hollow cathode arrangement 20 can be seen on the left side of FIG. It has two opposing targets 21. These targets are each plate-shaped, the plates being perpendicular to the image plane. A direct voltage of approximately 300 to 1,500 volts is applied between them. The entire arrangement, including the substrate 10, is in a spatial environment, not shown, in which there is a working pressure of approximately 0.05 to 5 hPa.
  • a noble gas stream, preferably argon stream, 22 is fed in on the left and flows between the two targets 21 to the right at a relatively high speed.
  • the plasma density decreases with increasing distance and, at preferred substrate positions at a distance of approximately 1 cm to 10 cm, is approximately 10 18 to 10 19 m "3.
  • This plasma density is approximately two orders of magnitude
  • the resulting intensive ion bombardment of the growing layer is to a large extent responsible for the good layer quality which can be achieved with this process even without applying a substrate bias
  • Production of hard Al 2 O 3 layers is that, in contrast to known magnitron sputtering processes, this process enables a high intensity of ionized species on the substrate, but the energy of the particles is very low and is only a few electron volts, which leads to the desired ion-induced Growth with minor growth disturbances in the layer that forms.
  • the material sputtered in the hollow cathode 20 is transported to the substrate 10 by the flow of the working gas, ie the argon flow 22. Diffusion overlaps this transport process. Due to the relatively high process pressure, neither a high vacuum pump nor the corresponding peripherals are required as a rule. This significantly reduces the system costs compared to other sputtering processes.
  • a combination of rotary vane and root pump can be used as the pumping station (not shown).
  • Oxygen O 2 is supplied as reactive gas 25 in the desired deposition of aluminum oxide.
  • the reactive gas is supplied outside the hollow cathode arrangement 20 in the process gas stream which is already widening there. If appropriate, the reactive gas can also be nitrogen or Contain carbon to separate admixtures of nitrides or carbides.
  • Diffusion of the reactive gas 25 between the targets 21 is prevented by the high flow velocity of the argon flow 22 as process gas. This avoids target poisoning that is known from other sputtering methods.
  • Sufficient reactive gas 25 is preferably used that no oxidation of the targets 21 takes place, not even at the edge regions 27. This can easily be determined by measuring methods (not shown) on the targets 21.
  • the process parameters can moreover be chosen largely independently of the data of the hollow cathode arrangement 20.
  • a displacement effect is also achieved on the substrate 10 by the intensive process gas stream (argon stream 22), which makes it possible to produce very pure layers even at relatively high residual gas pressures.
  • the deposition of layer material can be prevented by means of a shutter 26.
  • the substrate heater 12 can of course also achieve other temperatures of, for example, 400 ° C. to 1,000 ° C. for the substrates 10.
  • the parameters for the detailed adjustment of the properties of the deposited aluminum oxide layer are the target power, the intensity of the process gas flow, ie the argon flow 22, the amount of the supplied reactive gas 25, ie the reactive gas flow, the temperature of the substrate 10, the exact position of the Substrate 10 relative to the targets 21 of the hollow cathode arrangement, the total pressure and the process control.
  • a bias voltage can be applied between the substrate 10 or the holder of the substrate 10 and the hollow cathode arrangement as a source. This would lead to an expansion of the plasma zone from the source to the substrate 10.
  • indexable inserts made of hard metal P 20 of the type SNMA 120408 have been coated with aluminum oxide.
  • the indexable inserts were subjected to tenside cleaning and installed in the hollow cathode gas flow sputtering system.
  • the built-in substrate heater 12 the plates as substrate 10 were heated to 800 ° C.
  • the gas flow sputtering source which was coated with aluminum targets 21, was switched on and first operated with argon for five minutes. Thereafter, oxygen was introduced as the reactive gas 25 in the vicinity of the holder of the substrate 10 and the shutter 26 was opened after about three minutes. The coating takes place under constant conditions without substrate bias for 20 minutes. After this time, the shutter 26 was closed and the discharge and the supply of gases and the heating were switched off.
  • the substrates 10 were removed at a temperature of 100 ° C.
  • the layers were 5 ⁇ m thick and had a crystalline structure.
  • FIG. 2 shows a corresponding representation of the coated substrates 10 in which the alpha phase was determined by X-ray diffraction. There is a layer 11 on the substrate 10.
  • the layers which were produced using the method according to the invention were distinguished, inter alia, by the fact that the hardness was more than 1,800, even more than 2,000, measured by the Knoop method at a load of 0.025 pond.
  • the critical load at which layer 11 failed for the first time was greater than 80 N.
  • the structure was crystalline, the alpha phase was present, and layers 11 showed very good cutting behavior machining in the turning process of CK 45 steel.

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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)
  • Physical Vapour Deposition (AREA)

Abstract

L'invention concerne un procédé pour revêtir des substrats avec de l'oxyde d'aluminium (Al2O3), au moins une certaine proportion de cet oxyde étant en phase cristalline, procédé selon lequel les substrats sont revêtus par pulvérisation par flux de gaz avec cathode creuse, à des températures supérieures à 400 °C et inférieures à 1000 °C.
PCT/EP1998/005909 1997-09-16 1998-09-16 PROCEDE POUR REVETIR DES SUBSTRATS AVEC DE L'OXYDE D'ALUMINIUM (Al2O3) ET PIECE REVETUE SELON CE PROCEDE WO1999014393A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP98951423A EP1015654A1 (fr) 1997-09-16 1998-09-16 PROCEDE POUR REVETIR DES SUBSTRATS AVEC DE L'OXYDE D'ALUMINIUM (Al 2?O 3?) ET PIECE REVETUE SELON CE PROCEDE

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19740729.3 1997-09-16
DE19740729 1997-09-16
DE19830206A DE19830206C2 (de) 1997-09-16 1998-07-07 Verfahren zur Beschichtung von Substraten mit Aluminiumoxid (Al¶2¶O¶3¶)
DE19830206.1 1998-07-07

Publications (1)

Publication Number Publication Date
WO1999014393A1 true WO1999014393A1 (fr) 1999-03-25

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1998/005909 WO1999014393A1 (fr) 1997-09-16 1998-09-16 PROCEDE POUR REVETIR DES SUBSTRATS AVEC DE L'OXYDE D'ALUMINIUM (Al2O3) ET PIECE REVETUE SELON CE PROCEDE

Country Status (2)

Country Link
EP (1) EP1015654A1 (fr)
WO (1) WO1999014393A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI504773B (zh) * 2013-03-27 2015-10-21 Screen Holdings Co Ltd 氧化鋁之成膜方法及濺鍍裝置

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102021116727A1 (de) 2021-06-29 2022-12-29 Linde + Wiemann SE & Co. KG Verfahren zur Herstellung eines Profilbauteils aus einem rohrförmigen metallischen Halbzeug

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19518779C1 (de) * 1995-05-22 1996-07-18 Fraunhofer Ges Forschung Verbundkörper aus vakuumbeschichtetem Sinterwerkstoff und Verfahren zu seiner Herstellung

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19518779C1 (de) * 1995-05-22 1996-07-18 Fraunhofer Ges Forschung Verbundkörper aus vakuumbeschichtetem Sinterwerkstoff und Verfahren zu seiner Herstellung

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JUNG T ET AL: "Gas flow sputtering of oxide coatings: practical aspects of the process", 23RD INTERNATIONAL CONFERENCE ON METALLURGICAL COATINGS AND THIN FILMS, SAN DIEGO, CA, USA, 22-26 APRIL 1996, vol. 86-87, no. 1-3, ISSN 0257-8972, Surface and Coatings Technology, 1 Dec. 1996, Elsevier, Switzerland, pages 218 - 224, XP002092248 *
JUNG T ET AL: "HIGH RATE DEPOSITION OF ALUMINA FILMS BY REACTIVE GAS FLOW SPUTTERING", SURFACE AND COATINGS TECHNOLOGY, vol. 59, no. PART 01, 1 January 1993 (1993-01-01), pages 171 - 176, XP000576240 *
THORNTON J A ET AL: "STRUCTURE AND HEAT TREATMENT CHARACTERISTICS OF SPUTTER-DEPOSITED ALUMINA", AMERICAN CERAMIC SOCIETY BULLETIN., vol. 56, no. 5, May 1977 (1977-05-01), COLUMBUS US, pages 504 - 512, XP002092247 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI504773B (zh) * 2013-03-27 2015-10-21 Screen Holdings Co Ltd 氧化鋁之成膜方法及濺鍍裝置

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Publication number Publication date
EP1015654A1 (fr) 2000-07-05

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