Hard cubic Al-rich AlTiN coatings produced by PVD from ceramic targets

The PVD process using an arc evaporation method with an insulating ceramic target and controlled parameters produces Al-rich AlTiN coatings with a non-columnar microstructure, addressing the limitations of existing methods by achieving high hardness and wear resistance efficiently.

JP7796750B2Active Publication Date: 2026-01-09OERLIKON SURFACE SOLUTIONS AG PFAFFIKON
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Patent Information

Application Number
JP2023536373
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-12-16
Filing Date
2021-12-16
Publication Date
2026-01-09
Estimated Expiration
2041-12-16

AI Technical Summary

Technical Problem

Existing PVD methods for producing AlTiN coatings with high aluminum content face challenges such as prolonged coating times and the need for mild deposition conditions to achieve a pure cubic phase with columnar structure, which complicates the process and may lead to cracking.

Method used

A PVD process using an arc evaporation method with an insulating ceramic target and controlled nitrogen gas pressure and bias voltage to produce Al-rich AlTiN coatings with a non-columnar microstructure and high aluminum content, maintaining a stable arc discharge and cubic phase, even at low temperatures and pressures.

Benefits of technology

The method enables fast production of Al-rich AlTiN coatings with high hardness, compressive stress, and improved wear resistance, suitable for cutting tools, while ensuring excellent adhesion and stability.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

PVD coating process, preferably aluminum-rich Al X Ti 1-X 1. An arc evaporation PVD coating process for producing a thin film having an aluminum content of greater than 70 at-% based on the total amount of aluminum and titanium in the N-based thin film, a cubic structure, and an at least partially non-columnar microstructure having a non-columnar content of greater than 1 vol.% based on the volume of the total microstructure, the process comprising: a ceramic target having an aluminum-rich Al X Ti 1-X Used as a material source for N-based thin films in coating processes.
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Description

[Technical Field]

[0001] The present invention relates to a coating consisting of or including one or more hard cubic Al-rich AlTiN coating layers (hereinafter also simply referred to as hard cubic Al-rich AlTiN layers or hard cubic Al-rich AlTiN films) produced by a physical vapor deposition (PVD) process from a ceramic target, as well as a method for producing the same.

[0002] The hard cubic Al-rich AlTiN coating layer according to the present invention can be understood as a coating layer consisting of aluminum (Al), titanium (Ti) and nitrogen (N), or as a coating layer containing aluminum (Al), titanium (Ti) and nitrogen (N) as main components, and exhibiting a cubic crystal structure and a hardness of 30 GPa, preferably 35 GPa or more.

[0003] The term "exhibiting a cubic crystalline structure" can be understood to mean that the coating layer exhibits only the cubic phase, i.e., does not exhibit any hexagonal phase. However, this does not mean that the coating layer may have trace or small amounts of different phases, preferably less than 0.5% by weight relative to the total mass of the coating layer.

[0004] In this context, the use of the term "main components Al, Ti, N" in the context of an Al-rich AlTiN layer means that, when all elements contained in the Al-rich AlTiN layer are taken into consideration to determine the total chemical element composition of the Al-rich AlTiN layer in atomic percentages, the sum of the contents of Al, Ti and N in the Al-rich AlTiN layer as concentrations in atomic percentages is greater than 50 at% (i.e., a value between 50 at% and 100 at%), preferably greater than 75 at% (i.e., a value between 75 at% and 100 at%), and more preferably equal to or greater than 80 at% (i.e., a value between 80 at% and 100 at%).

[0005] In this context, the term "Al-rich" may be used in particular to indicate that the content of aluminum (Al) in the corresponding Al-rich AlTiN layer is equal to or preferably exceeds 70 at% when only Al and Ti are considered for determining the chemical element composition in atomic percentage (i.e., Al [at%] / Ti [at%] ≥ 70 / 30). [Background technology]

[0006] technical level AlTiN coating layers with an Al content of more than 75 at.-% (relative to Ti) exhibiting cubic and columnar microstructures are known to be synthesized by LP-CVD processes. These types of coatings are also known as PVD-based Al 0.67 Ti 0.33 It is known to exhibit superior wear protection compared to coatings with lower Al content, such as N coatings.

[0007] Historically, it has been well known that PVD methods such as arc evaporation and reactive magnetron sputtering can be used to produce AlTiN layers in the metastable cubic (B1 crystal structure) phase with up to 70 at.-% Al.

[0008] Furthermore, several publications have presented possible methods for increasing the metastable solubility limit of Al beyond 70 at.%. However, all of these methods proposed so far have some drawbacks or limitations. One limitation, for example, is the deposition of only the cubic phase with a columnar structure, which increases the coating effort, especially the coating time. Furthermore, when depositing exclusively the cubic phase with a columnar structure, care must be taken to ensure that the deposition conditions are particularly mild. Summary of the Invention [Problem to be solved by the invention]

[0009] Object of the invention It is an object of the present invention to provide a method for producing hard cubic Al-rich AlTiN coating layers that overcomes or mitigates the drawbacks or limitations of the state of the art.

[0010] The hard cubic Al-rich AlTiN coating should preferably exhibit 100% cubic phase, high hardness, suitable compressive stress, and coating microstructure, which allows the Al-rich AlTiN coating to preferably achieve high wear resistance and improved cutting performance when applied to cutting tools. Furthermore, the coating layer according to the present invention should be simple and fast to produce. [Means for solving the problem]

[0011] Description of the invention The object of the present invention is achieved by providing a coating comprising at least one hard cubic Al-rich AlTiN coating layer as described below and as claimed in claim 10, and a method for producing the same as described below and as claimed in claim 1.

[0012] In a first aspect of the present invention, a PVD coating process, preferably an aluminum-rich Al X Ti 1-X 1. An arc evaporation PVD coating process for producing a thin film having an aluminum content of greater than 70 at-% based on the total amount of aluminum and titanium in the N-based thin film, a cubic structure, and an at least partially non-columnar microstructure having a non-columnar content of greater than 1 vol.% based on the volume of the total microstructure, the process comprising: a ceramic target having an aluminum-rich Al X Ti 1-X A coating process is disclosed that is used as a material source for N-based thin films.

[0013] In another example of the first aspect, an arc evaporation PVD coating process is used as the PVD coating process.

[0014] In another example of the first embodiment, aluminum-rich Al X Ti1-X The N-based thin film may have a mixed columnar and non-columnar microstructure, with the non-columnar microstructure content being greater than 1% by volume, preferably greater than 20% by volume, and particularly greater than 50% by volume.

[0015] In another example of the first embodiment, an aluminum-rich Al alloy having a non-columnar microstructure is X Ti 1-X N-based thin film.

[0016] Furthermore, in another example of the first embodiment, a brittle insulating ceramic target is used. In another example of the first embodiment, an arc current of preferably greater than 80 amperes may be used, and in particular an arc current of between 80 and 200 amperes may be used.

[0017] In another example of the first aspect, at least one target includes additional insulation in the center, and the arc steering is operated to prevent the ceramic target from cracking during arcing.

[0018] In another example of the first embodiment, Al X Ti 1-X N may be used as a target material, and X may be 75 or more, and preferably X may have a value between 75 and 90.

[0019] Additionally, in another example of the first aspect, the at least one ceramic target remains 99% dense and crack-free during processing.

[0020] In another example of the first embodiment, Al X Ti 1-X N may be used as the target material, and the AlN content may be greater than 70% by volume of the target material, preferably greater than 75% by mole.

[0021] In another example of the first embodiment, nitrogen may be introduced as the reactive gas, preferably at a pressure of less than 0.5 Pa, in particular between 0.3 and 0.1 Pa.

[0022] In another example of the first aspect, a negative bias voltage may be applied to the substrate to be coated, and the bias voltage applied to the substrate may preferably range between -250V and -30V, more preferably between -200V and -80V, and especially between -200V and -100V.

[0023] In another example of the first embodiment, the deposition temperature during the coating process may be below 360°C, preferably between 150°C and 320°C.

[0024] In another example of the first embodiment, a plurality of aluminum-rich Al X Ti 1-X Multilayer films can be fabricated by depositing N-based thin films on top and bottom, and Al exhibits a non-columnar microstructure despite its cubic structure. X Ti 1-X The N content varies with respect to adjacent layers.

[0025] In a second aspect of the present invention, aluminum-rich Al x Ti 1-x An aluminum-rich AlN-based thin film producible by a process according to the first aspect of the present invention, the aluminum-rich AlN thin film having an aluminum content of greater than 70 at-% based on the total amount of aluminum and titanium in the film, a cubic crystal structure, and an at least partially non-columnar microstructure having a non-columnar content of greater than 1 vol.% based on the total microstructure. x Ti 1-x N-based thin films are disclosed.

[0026] In another example of the second embodiment, aluminum-rich Al X Ti 1-XThe N-based thin film may have a mixed columnar and non-columnar microstructure, with the non-columnar microstructure content being greater than 1% by volume, preferably greater than 20% by volume, and particularly greater than 50% by volume.

[0027] In another example of the second embodiment, the thin film may contain Al, Ti, and N as the major components, and may be represented by the formula (Al a Ti b ) x N y where a and b are the concentrations of aluminum and titanium, respectively, in atomic ratio, considering only Al and Ti for the calculation of the chemical elemental composition in the layer, where a+b=1, and 0≠a≧0.7 and 0≠b≧0.2, or 0≠a≧0.8 and 0≠b≦0.2; x is the concentration of Al plus the concentration of Ti; and y is the concentration of nitrogen, in atomic ratio, considering only Al, Ti, and N for the calculation of the elemental composition in the layer, where preferably x+y=1, and 0.45≦x≦0.55.

[0028] In another example of the second embodiment, the thin film may exhibit a hardness of 30 GPa or greater, preferably 35 GPa or greater, measured using instrumented indentation according to ISO 14577-1.

[0029] In another example of the second embodiment, the thin film may exhibit a reduced Young's modulus in the range of between 350 GPa and 480 GPa, preferably in the range of between 370 GPa and 410 GPa, measured using instrumented indentation in accordance with ISO 14577-1.

[0030] In another example of the second embodiment, the thin film can exhibit a compressive stress of greater than 2.5 GPa, preferably in the range of between 2.5 GPa and 6 GPa, measured using instrumented indentation in accordance with ISO 14577-1.

[0031] In another example of the second embodiment, the thin film exhibits high adhesion of HF1 even at a coating thickness of 5 μm, which high adhesion results particularly from the deposition of the thin film by the combination of the use of a ceramic target and arc discharge.

[0032] In another example of the second embodiment, aluminum-rich Al X Ti 1-X The N-based thin film is made of multiple aluminum-rich Al films deposited on top and bottom. X Ti 1-X It can be formed as a multilayer film including an N-based thin film, and preferably an Al-based thin film that can exhibit a non-columnar microstructure. X Ti 1-X The N content may vary for adjacent layers.

[0033] In another example of the second embodiment, the thin film may have an aluminum content of X≧75, preferably an aluminum content of X between 75-90.

[0034] In another example of the second embodiment, the layer thickness may be greater than 500 nm, preferably greater than 1000 nm, in particular greater than 1500 nm.

[0035] In a third aspect of the present invention, there is provided a method for producing a coated tool or coated component, in particular a coated cutting tool or coated forming tool, or a coated turbine component or coated component used in wear-resistant applications, using an aluminium-rich Al alloy according to the second aspect of the present invention. x Ti 1-x The use of N-based thin films is disclosed.

[0036] As at least partially described above, and to summarize some important aspects of the present invention, the present invention is particularly directed to a ferroelectric material comprising, as major components, Al, Ti, and N, and having the formula (Al a Ti b ) x N ywherein a and b are the concentrations of aluminum and titanium, respectively, in atomic ratio, taking into account only Al and Ti for the calculation of the elemental composition in the layer, a+b=1, and 0≠a≧0.7 and 0≠b≧0.2, or 0≠a≧0.8 and 0≠b≦0.2, x is the sum of the concentrations of Al and Ti, and y is the concentration of nitrogen, in atomic ratio, taking into account only Al, Ti, and N for the calculation of the elemental composition in the layer, x+y=1, and 0.45≦x≦0.55, The coating layer may exhibit: o 100% fcc cubic phase, oHardness H≧35GPa, a reduced Young's modulus Er in the range between 350 GPa and 480 GPa, i.e., 350 GPa≦Er≦480 GPa, more preferably in the range between 370 GPa and 410 GPa, i.e., 370 GPa≦Er≦410 GPa;

[0037]

number

[0038] Hardness and reduced modulus are measured using instrumented indentation in accordance with ISO 14577-1 test method.

[0039] o Compressive stress of 2.5 GPa or more, preferably between 2.5 GPa and 6 Pa. o Either a columnar or non-columnar structure, or a structure consisting of a continuous stack of columnar and non-columnar modulated layers, while having a 100% cubic phase with a composition of AlTiN greater than 0.7 moles of AlN.

[0040] The compressive stress between o4 and 6 GPa and the adhesive properties of HF1 are simultaneously demonstrated even at a coating thickness of 5 μm.

[0041] Furthermore, the present invention particularly relates to a method for producing a coating layer according to the first aspect of the invention on the surface of a substrate, The coating layer may be formed inside a vacuum coating chamber by using PVD cathodic arc evaporation techniques, in particular at least one arc evaporation source may be used, comprising a target of insulating ceramic material, in particular a target made of insulating AlN with a mole fraction of more than 70%, acting as a cathode for evaporating the target material; The target material may consist of Al, Ti and N or may contain Al, Ti and N as main components, in particular If only the contents of Al, Ti and N in atomic percentage in the target material are considered, the formula (Al c Ti d ) t N z where c and d are the concentrations of aluminum and titanium, respectively, in atomic ratio, considering only Al and Ti for the purpose of calculating the elemental composition in the layer, and c+d=1, c / d≧70 / 30, and 0≠c≧0.7 and 0≠d≧0.10; t is the sum of the concentrations of Al and Ti; and z is the nitrogen concentration, in atomic ratio, considering only Al, Ti, and N for the purpose of calculating the elemental composition in the layer, and t+z=1, and 0.45≦z≦0.55, preferably z=0.5; The method may further comprise the deposition of aluminum titanium nitride from an insulating ceramic target, wherein nitrogen gas is introduced into the vacuum coating chamber to compensate for the loss of nitrogen provided by the target during the coating process; - Vapor deposition of titanium aluminum nitride At a deposition temperature below 360°C, preferably between 150°C and 320°C, At a nitrogen partial pressure of less than 0.5 Pa, preferably between 0.1 Pa and 0.3 Pa, o performed using a bias voltage Ub in the range corresponding to -250 V ≦ Ub ≦ -30 V, preferably in the range corresponding to -200 V ≦ Ub ≦ -80 V, more preferably in the range corresponding to -200 V ≦ Ub ≦ -100 V, The insulating ceramic target may include an insulator within the insulating target, as proposed by Krassnitzer in PCT / EP2020 / 068828. Surprisingly, this configuration made it possible to maintain a stable arc discharge over a wide range of currents, i.e., from 80 A to 200 Amp, even though the target had a mole fraction of insulating material greater than 70%.

[0042] Stable arc discharge on insulating ceramic targets at low operating pressures below 0.2 Pa.

[0043] Therefore, to enable arc discharge of the ceramic target and achieve a stable arc discharge, the method can preferably be carried out by using one or more arc evaporation sources, as described by Krassnitzer in PCT / EP2020 / 068828. In this way, it is possible to carry out a reactive PVD coating process and produce an Al-rich AlTiN coating layer (having an Al content of more than 75 at%, as explained above) such that an arc current of, for example, 200 A can be applied to the ceramic target, and at the same time a discharge voltage of more than 30 V can be achieved in the arc discharge, while maintaining a power contribution of less than 20% that leads to substrate heating.

[0044] The preferred AlTiN with Al>75% can be grown with a cubic structure and high hardness at low temperature, low gas pressure (high energy input from the ions) and high bias voltage.

[0045] The inventors have found that the combination of Al and Ti in the above-mentioned ratios in the Al-rich AlTiN-layer, meaning Al[at%] / Ti[at%]≧70 / 30, preferably Al[at%] / Ti[at%]>70 / 30, more preferably 90 / 10≧Al[at%] / Ti[at%]≧75 / 25, shows a significant contribution to improving the wear protection of the tool and / or component.

[0046] Furthermore, the present invention particularly relates to coating systems comprising one or more hard cubic Al-rich AlTiN coating layers of the present invention.

[0047] The above inventive method for producing the above inventive hard cubic Al-rich AlTiN coating layer can also be modified, for example by using additional targets and / or reactive gas flows, to produce other types of coating layers that are combined with the inventive hard cubic Al-rich AlTiN coating layer to produce different coating systems, for example multilayer and / or gradient coating systems.

[0048] The Al-rich AlTiN coating layer and / or coating system according to the present invention (i.e., including the Al-rich AlTiN coating layer according to the present invention) is expected to exhibit excellent mechanical properties and have a beneficial set of characteristics for providing excellent performance in tools and components subjected to wear and stress accumulation.

[0049] The above-mentioned (Al a Ti b ) x N y The layer can exhibit a 100% face-centered cubic (fcc) structure. Importantly, the present invention describes a method for producing the Al-rich AlTiN coatings of the present invention by a physical vapor deposition (PVD) process, specifically by arc-discharging an insulating ceramic AlTiN target(s) containing AlTiN, particularly having greater than 70 at% Al relative to Ti, and by simultaneously introducing controlled N gas into a vacuum coating chamber (also referred to as a PVD apparatus). Furthermore, the present invention demonstrates how to synthesize Al-rich AlTiN in both columnar and non-columnar structures while retaining only the cubic phase despite the high AlN fraction. Surprisingly, thin films synthesized using insulating ceramic targets also exhibit superior adhesion to substrates compared to those synthesized using metal targets, as shown in Figure 9.

[0050] Detailed Description In order to provide a better understanding of the present invention, some examples, tables and figures are used below to describe the present invention in more detail. However, these examples, tables and figures should not be understood as limitations of the present invention, but should be understood only as specific examples and / or preferred embodiments of the present invention.

[0051] As described below, inventive examples of hard cubic Al-rich AlTiN layers deposited according to the present invention were carried out using a cathodic arc evaporation process at a process temperature of 300°C (in this context, the term "process temperature" is used to refer specifically to the set temperature during the coating deposition process) and a low nitrogen partial pressure between 0.2 Pa and 0.15 Pa. (Al 0.77 Ti 0.23 ) 0.5 N 0.5 A target having the chemical element composition of was used, and the target was operated as a cathode by applying an arc current of 80 A to 200 A, a substrate bias voltage of −120 V, and a nitrogen partial pressure between 0.15 Pa and 0.20 Pa.

[0052] Two inventive examples of such inventive deposition processes with detailed process parameters and measured coating layer properties deposited in these inventive examples are shown in Tables 1.1 and 1.2.

[0053] Three comparative examples of deposition processes not of the present invention with detailed process parameters and measured coating layer properties deposited in these comparative examples are listed in Tables 2.1 and 2.2.

[0054] SEM and X-ray examinations of the hard cubic Al-rich AlTiN coatings of the present invention obtained by the coating processes shown in Inventive Examples 1-2 are shown in Figures 1-4.

[0055] SEM and X-ray examinations of Al-rich AlTiN coatings not according to the invention obtained by the coating processes shown in Comparative Examples 3-5 are shown in Figures 5-10.

[0056] drawing: [Brief explanation of the drawings]

[0057] [Figure 1] 1 is an SEM fracture cross-section image of a hard cubic Al-rich AlTiN coating deposited according to Inventive Example 1. [Figure 2] 1 is an SEM fracture cross-section image of a hard cubic Al-rich AlTiN coating deposited according to Inventive Example 1. [Figure 3] 1 shows X-ray patterns of as-deposited hard cubic Al-rich AlTiN coatings deposited according to inventive examples 1 and 2. [Figure 4] 10 is an SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 3. [Figure 5] 10 is an SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 4. [Figure 6] 10 is an SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 5. [Figure 7] 10 shows X-ray patterns of as-deposited Al-rich AlTiN coatings deposited according to Comparative Examples 3, 4, and 5. [Figure 8] Ceramic targets adapted for reliable operation as cathodes in cathodic arc evaporation sources. [Figure 9] X-SEM (a) and coating resistance to delamination under HRC indentation (b) of inventive coatings (#2620, #3007) and comparative (#2301) coatings. DETAILED DESCRIPTION OF THE INVENTION

[0058] [Table 1]

[0059] [Table 2]

[0060] [Table 3]

[0061] [Table 4]

[0062] Film structure analysis was performed by X-ray diffraction (XRD) using a PANalytical X'Pert Pro MPD diffractometer equipped with a CuKa radiation source. Diffraction patterns were collected in Bragg-Brentano geometry. Micrographs of film fracture cross sections were obtained using a FEGSEM Quanta F 200 Scanning Electron Microscope (SEM).

[0063] The hardness and indentation modulus of the as-deposited samples were determined using an Ultra-Micro-Indentation System equipped with a Berkovich diamond tip. The test procedure involved a normal load of 10 mN. Hardness values ​​were evaluated according to the Oliver and Pharr method. Thereby, we ensured an indentation depth of less than 10% of the coating thickness to minimize substrate interference.

[0064] As shown in Table 1.2, it exhibits a predominantly columnar microstructure, but with at least 1% by weight of non-columnar microstructure, already allowing for easy coating.

[0065] drawing: FIG. 1: SEM fracture cross-section image of a hard cubic Al-rich AlTiN coating deposited according to inventive example 1.

[0066] FIG. 2: SEM fracture cross-section image of a hard cubic Al-rich AlTiN coating deposited according to inventive example 1.

[0067] FIG. 3: X-ray patterns of as-deposited hard cubic Al-rich AlTiN coatings deposited according to inventive Examples 1 and 2.

[0068] FIG. 4: SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 3.

[0069] FIG. 5: SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 4.

[0070] FIG. 6: SEM fracture cross-section image of an Al-rich AlTiN coating deposited according to Comparative Example 5.

[0071] FIG. 7: X-ray patterns of as-deposited Al-rich AlTiN coating films deposited according to Comparative Examples 3, 4, and 5.

[0072] Figure 8: Ceramic target adapted for reliable operation as a cathode in a cathodic arc evaporation source.

[0073] Figure 9: X-SEM (a) and the coating of the present invention Gu( Coating resistance to delamination under HRC indentation for (#2620, #3007) and comparative (#2301) coatings (b).

[0074] To produce the inventive Al-rich AlTiN-based films and tunable microstructures, the inventors used an arc evaporation process on an insulating ceramic target having a minimum of 70 at% Al relative to the Ti content, where the inventive combination of deposition parameters was selected based on the following understanding: a) At the target: The arc discharge current, magnetic field distribution and strength are selected to form the desired plasma state of film-forming species consisting of singly and multiply charged ions of Al, Ti and N, and the arc current is varied between 80 A and 200 A to switch the microstructure between columnar and non-columnar structures.

[0075] b) At the substrate: The bias voltage is high enough to increase the kinetic energy, thereby increasing the quenching rate of the incident ions at the thin film growth surface. At the same time, the substrate temperature is low enough to freeze the adatom mobility on the growth surface.

[0076] c) General: The nitrogen gas pressure is operated within a desired window that is low enough to reduce the collection of nitrogen ions, thereby suppressing the nucleation of the hexagonal phase enabled by the gas ion-induced remixing effect on the growth surface, and the nitrogen gas pressure is high enough to form stoichiometric AlTiN thin films.

[0077] By optimizing the above process levels of arc evaporation, the nucleation of the thermodynamically favored hexagonal phase was suppressed at the growth surface, thereby increasing the metastable solubility of Al in c-AlTiN to concentrations greater than 75 at.% (e.g., 80 at.%). Furthermore, surprisingly, the microstructure could be tuned between columnar and non-columnar while retaining a single-phase cubic solid solution.

[0078] Specific advantages of the present invention The present invention provides a method that allows: Al 77 Ti 23 N or, for example, Al 90 Ti 10 Synthesis of stoichiometric and cubic Al-rich AlTiN thin films by arc evaporation of ceramic targets further containing higher Al content relative to Ti up to a composition of N.

[0079] Selection of parameters for stable arc discharge of a ceramic target with a volume fraction of semiconductor AlN exceeding 70% by using nitrogen gas pressures below 0.2 Pa. Generally, it is difficult to maintain smooth arc movement at such low gas pressures. However, the ceramic target used in accordance with the present invention facilitates low-pressure operation.

[0080] Al 77 Ti 23N or, for example, Al 90 Ti 10 Synthesis of both columnar and non-columnar cubic phase solid solutions further containing higher contents of Al relative to Ti up to a composition of N.

[0081] Synthesis of Al-rich AlTiN films processed via ceramic targets that exhibit superior resistance to HRC indentation-induced delamination compared to thin films processed via metallic targets.

[0082] Arc discharge of an insulating ceramic target for producing a coating having a composition of AlTiN with an AlN content of more than 75 mol%, wherein deposition is possible by using a wide range of arc currents between 80 A and 200 A and maintaining a stable arc discharge at a low gas pressure of less than 0.2 Pa.

[0083] Synthesis of AlTiN with cubic structure and AlN contents above 75 mol% in both columnar and non-columnar microstructures and even as modulated layers of columnar and non-columnar structures.

[0084] Synthesis of AlTiN with a cubic structure and an AlN content of more than 75 mol% in both columnar and non-columnar microstructures, deposited by Arc evaporation from an insulating ceramic target, where the deposited coating exhibits very good adhesion to the substrate (HF1) despite compressive stresses as high as 5 GPa and thicknesses as high as 5 μm.

Claims

1. Aluminum-rich Al x Ti 1-x 1. An arc evaporation PVD coating process for producing a thin film on a substrate having an aluminum content of greater than 70 at-%, based on the total amount of aluminum and titanium in the N-based thin film, a cubic crystal structure, and an at least partially non-columnar microstructure having a non-columnar content of greater than 1 vol. %, based on the volume of the total microstructure, wherein a ceramic target is used to coat the aluminum-rich Al x Ti 1-x It is used as a material source for N-based thin films, An arc current of between 80 amps and 200 amps is used; Nitrogen is introduced as a reactive gas, the nitrogen being introduced at a pressure between 0.3 and 0.1 Pa; A negative bias voltage (U b ) is applied to the substrate, and the negative bias voltage (U b ) applied to the substrate is in the range between −250 V and −30 V; A coating process wherein the deposition temperature during said coating process is between 150°C and 320°C.

2. The aluminum-rich Al x Ti 1-x The N-based thin film has a mixed columnar and non-columnar microstructure, the non-columnar microstructure having a content of more than 1% by volume, preferably more than 20% by volume, and particularly more than 50% by volume. The coating process of claim 1.

3. The aluminum-rich Al x Ti 1-x 3. The coating process of claim 1 or 2, wherein the N-based thin film has a non-columnar microstructure.

4. An insulating ceramic target is used. The coating process according to any one of claims 1 to 3.

5. At least one target is provided with an additional insulator in the center, and arc steering is operated to prevent cracking of the ceramic target during arc discharge. A coating process according to any one of claims 1 to 4.

6. Al x Ti 1-x N is used as the target material, and X is 75 or more, preferably having a value between 75 and 90; A coating process according to any one of claims 1 to 5.

7. At least one ceramic target remains 99% dense and crack-free during processing; A coating process according to any one of claims 1 to 6.

8. Al x Ti 1-x N is used as a target material, and the AlN content is more than 70 vol. %, preferably more than 75 mol. % of the target material; A coating process according to any one of claims 1 to 7.

9. The negative bias voltage (U b ) is in the range of −200 V to −80 V, in particular −200 V to −100 V; A coating process according to any one of claims 1 to 8.

10. Multiple aluminum-rich Al x Ti 1-x A multilayer film is fabricated by depositing N-based thin films on top and bottom, and Al exhibits a non-columnar microstructure despite its cubic structure. x Ti 1-x The N content varies with respect to adjacent layers; A coating process according to any one of claims 1 to 9.

11. Aluminum-rich Al x Ti 1-x An N-based thin film having an aluminum content of greater than 70 at-% based on the total amount of aluminum and titanium in the film, a cubic crystal structure, and an at least partially non-columnar microstructure having a non-columnar content of greater than 1 vol.% based on the total microstructure; the thin film exhibits a hardness (H) of 30 GPa or greater, measured using instrumented indentation according to ISO 14577-1; and / or the thin film exhibits a Young's modulus (E r ) in the range between 350 GPa and 480 GPa, measured using instrumented indentation according to ISO 14577-1; and / or the thin film exhibits a compressive stress of greater than 2.5 GPa, as measured using instrumented indentation in accordance with ISO 14577-1; x Ti 1-x N-based thin film.

12. The aluminum-rich Al x Ti 1-x The N-based thin film has a mixed columnar and non-columnar microstructure, the non-columnar microstructure having a content of more than 1% by volume, preferably more than 20% by volume, and particularly more than 50% by volume. The aluminum-rich Al according to claim 11 x Ti 1-x N-based thin film.

13. The thin film contains Al, Ti, and N as main components and has a formula (Al a Ti b ) x N y wherein a and b are the concentrations of aluminum and titanium, respectively, in atomic ratio, taking into account only Al and Ti for the calculation of the chemical element composition in the layer, where a+b=1, and 0≠a≧0.7 and 0≠b≧0.2, or 0≠a≧0.8 and 0≠b≦0.2, x is the concentration of Al plus the concentration of Ti, and y is the concentration of nitrogen, in atomic ratio, taking into account only Al, Ti and N for the calculation of the chemical element composition in the layer, where preferably x+y=1, and 0.45≦x≦0.

55. The aluminum-rich Al according to claim 11 or 12 x Ti 1-x N-based thin film.

14. The aluminum-rich Al thin film according to any one of claims 11 to 13, wherein the thin film exhibits a hardness (H) of 35 GPa or more, measured using instrumented indentation according to ISO 14577-1. x Ti 1-x N-based thin film.

15. The thin film has a Young's modulus (E) in the range between 370 GPa and 410 GPa, measured using instrumented indentation according to ISO 14577-1. r 15. The aluminum-rich Al alloy according to claim 11, wherein x Ti 1-x N-based thin film.

16. 16. The aluminum-rich Al thin film according to any one of claims 11 to 15, wherein the thin film exhibits a compressive stress ranging between 2.5 GPa and 6 GPa, measured using instrumented indentation according to ISO 14577-1. x Ti 1-x N-based thin film.

17. 17. The aluminum-rich Al thin film according to claim 11, wherein the thin film exhibits high adhesion of HF1 even at a coating thickness of 5 μm, and this high adhesion results in particular from the deposition of the thin film by the use of a ceramic target in combination with arc discharge. x Ti 1-x N-based thin film.

18. The aluminum-rich Al x Ti 1-x N-based thin films are deposited on top and bottom of multiple aluminum-rich Al x Ti 1-x The Al thin film is formed as a multilayer film including an N-based thin film, and preferably exhibits a non-columnar microstructure. x Ti 1-x The aluminum-rich Al alloy according to any one of claims 11 to 17, wherein the N content varies with respect to adjacent layers. x Ti 1-x N-based thin film.

19. 19. Aluminium-rich Al thin film according to any one of claims 11 to 18, wherein the thin film has an aluminium content of X≧75, preferably between 75 and 90. x Ti 1-x N-based thin film.

20. The aluminum-rich Al film according to claim 11, wherein the layer thickness is greater than 500 nm, preferably greater than 1000 nm, in particular greater than 1500 nm. x Ti 1-x N-based thin film.

21. 21. The aluminum-rich Al alloy according to claim 11, for producing coated tools or coated components, in particular coated cutting tools or coated forming tools, or coated turbine components or coated components used in wear-resistant applications. x Ti 1-x Use of N-based thin film.

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