ICMCTF2007 Session B5-2: Properties and Characterization of Hard Coatings and Surfaces

Monday, April 23, 2007 1:30 PM in Room Golden West

Monday Afternoon

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1:30 PM B5-2-1 Industrial Perspective on Characterization of Hard Coatings for Cutting Tool Applications
Y. Tanaka, K. Sato (Mitsubishi Materials Corporation, Japan); N. Ichimiya (Mitsubishi Materials Kobe Tools Corporation, Japan)
In order to cope with the higher efficient cutting tool applications, variety types of PVD coatings are proposed and widely used, where mechanical and oxidation properties of the coating have been drawn the most attention as wear resistance characteristics of the cutting tools. In this paper, Al-Ti-N and Al-Ti-Si-N coatings were deposited on WC-Co and platinum substrates by using the cathodic arc ion plating method and microstructure-property relationship, characterized by XRD, TEM, XPS, indentation tests and ball-on-disk wear tests, was discussed in terms of the performance of cutting tools. The residual stress of the Al-Ti-N coatings was found to vary significantly with the negative bias voltages. The changes in microstructure were related to the film strains induced by ion bombardment. At higher bias voltages, the films were mainly composed of granular structures and with the decrease of negative substrate bias voltage, the microstructure changed to a columnar structure. Cutting performance of Al-Ti-N coated carbide drills were investigated and the results were discussed with the microstructure and properties of the Al-Ti-N coatings. The Al-Ti-Si-N coatings with cubic B1 nano crystal structures had higher hardness than Al-Ti-N coatings. Similarly, the addition of Si to Al-Ti-N coatings improved the oxidation resistance and Al-Ti-Si-N coatings displayed greatly improved oxidation resistance at elevated temperatures in air. Microstructure and composition evolution of the local area of the Al-Ti-Si-N coatings heat treated at elevated temperatures were also investigated and the results were discussed with the oxidation resistance property. Al-Ti-Si-N coated carbide endmills were evaluated and offered significantly better performance in the machining of hardened steels with the high cutting speeds. Wear mechanism and cutting characteristics were discussed with the film properties.
2:10 PM B5-2-3 Properties and Cutting Performance of AlTiCrN/TiSiCN Bilayer Coatings Deposited by Cathodic Arc Ion Plating
S. Imamura, H. Fukui, A. Shibata, N. Omori (Sumitomo Electric Hardmetal Corp., Japan); M. Setoyama (Sumitomo Electric Industries, Ltd., Japan)
This study was intended to investigate the properties and cutting performance of AlTiCrN/TiSiCN bilayer coatings. These coatings were deposited on cemented carbide substrate by the cathodic arc ion plating method, using AlTiCr and TiSi alloy source. The properties of these coatings were investigated by nano-indentation, X-ray diffraction (XRD), pin-on-disc test, selected ion monitoring (SIM), transmission electron microscopy (TEM) and X-ray photoelectron spectrometer (XPS). Nano indentation hardness of AlTiCrN and TiSiCN were 41GPa and 51GPa, respectively. AlTiCrN layer was columnar structure and its size was less than 50nm. On the other hand, TiSiCN layer was nano crystalline structure and its size was about 5nm. In particular, TiSiCN film showed good tribological behavior and its friction coefficient was 0.18 for the bearing steel counterparts (AISI 52100). AlTiCrN/TiSiCN bilayer coated carbide endmills were evaluated in the machining of carbon steel (AISI 1049), hardened steel (AISI D2) and gray cast iron (AISI 35). These coated endmills showed better wear resistance than TiAlN coated endmills. The good tribological properties of TiSiCN layer decreased adhesion. However, the cutting performance of mono layer TiSiCN coated endmill was not so good because of high compressive residual stress. AlTiCrN/TiSiCN bilayer coatings showed excellent cutting performance for all kind of work materials.
2:30 PM B5-2-4 Effect of Film Deposition Time on the Mechanical Properties and Cutting Performance of Coated Tools
K.-D. Bouzakis, G. Skordatis, N. Michailidis (Aristoteles University of Thessaloniki, Greece); G. Erkens (Metaplas Ionon, Germany)

PVD process parameters such as deposition duration, bias voltage etc., affect significantly film strength properties and through them the coated tool cutting performance. In the described investigations, cemented carbide inserts were coated with nanocomposite (Ti45Al55)N films through high ionization sputtering (HIS) PVD processes by plasma booster technology, keeping all process parameters constant in the vacuum chamber except the deposition time.

To compare the cutting performance of inserts of the same TiAlN PVD films and coating thickness, the film deposition was performed as follows. Cemented carbide specimens were placed in various locations in the vacuum chamber simultaneously with further items to be coated, so that due to shadowing effects the plasma flux was variable. As a result in PVD processes of an overall duration of 14400 sec and of 5400 sec respectively, inserts with various thicknesses were produced according to their location in the vacuum chamber. Coated cutting inserts with a film thickness of approximately 2.7 µm, originated from both the aforementioned PVD processes, with various overall deposition times were employed.

The characterization of the films' strength properties was performed through nanoindentation and a finite element methods (FEM) supported evaluation of the corresponding measurement results. Impact tests were carried out to determine film fatigue properties. The cutting performance of the coated inserts was investigated systematically in milling. The obtained results were explained by FEM simulation of the cutting process, considering the mechanical and fatigue properties, established by nanoindentations and impact tests as described before. The results revealed that longer deposition times improve the yield, rapture and critical fatigue stress, resulting to a significant tool life increase.

2:50 PM B5-2-5 A Study on the Microstructures and Mechanical Properties of Pulsed DC Reactive Magnetron Sputtered Cr-Si-N Nanocomposite Coatings
J.-W. Lee, Y.C. Chang (Tung Nan Institute of Technology, Taiwan)
The nanocomposite Cr-Si-N thin films with various Si contents have been deposited by a bipolar asymmetric pulsed DC reactive magnetron sputtering system. The Cr-Si-N thin films with Si contents ranging from 0.3 at.% to 15.1 at.% were achieved. The structures of Cr-Si-N films were characterized by XRD. The surface and cross sectional morphologies of thin films were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The surface roughness of thin films was explored by atomic force microscopy (AFM). The nanoindentation, nanoscratch and nanowear tests were adopted to evaluate the nanomechanical properties of Cr-Si-N coatings. The crystalline CrN is observed to be the main phase in the Cr-Si-N thin films. A high hardness, low scratch coefficient and good wear resistance properties are found in the coatings with around 7 to 9 at.% Si in this work.
3:10 PM B5-2-6 Cracking and Failure Behaviour of Nitride Coatings
J.S. Colligon (Manchester Metropolitan University, United Kingdom); B.D. Beake (Micro Materials Ltd., United Kingdom); V.M. Vishnyakov (Manchester Metropolitan University, United Kingdom); R. Valizadeh (Manchester Metropolitan University, Untied Kingdom)

TiN/Si3N4, TiFeN and TiFeN/Mo films were produced on silicon substrates using a dual ion beam system. Mechanical properties have been determined by nano-indentation and tribological properties have been measured by nano-scratch testing. The nano-indentation showed that harder nitrides exhibited higher ratios of hardness to modulus (H/E). The dependence of the resistance to plastic deformation (H3/E2) on hardness was approximately linear.

When applying a load, which increases linearly with distance, the distance to the start of cracks (first cohesive failure) lc1 and the distance to total delamination lc2 can be expressed as a ratio T = (lc2 - lc1)/lc1. The ratio can be treated as a measure of the specific coating/substrate toughness (SCT). This SCT is seen to correlate well with the ratio H/E. The SCT appears to give a better correlation with H/E than the crack propagation resistance (lc2 - lc1) x lc1 defined earlier by Zhang at al.1

It is shown by our data that use of the SCT enables comparison of data on films of different thickness and/or using probe of differing radius. Data from a wide range of different film-substrate systems have been evaluated and correlations with H/E investigated and optimum H/E values for enhanced durability determined.

1 Zhang S, Sun D, Fu Y and Du H, Thin Solid Films 447-8, 462 (2004)}

3:30 PM B5-2-7 Abrasive Wear of Textured-Controlled CVD Al2O3 Coatings
M. Fallqvist, M. Olsson (Dalarna University, Sweden); S. Ruppi (SECO Tools, Sweden)

Today cemented carbides are the dominant tool material for metal cutting using indexable inserts. For these, coatings of hard refractory materials such as TiC, Ti(C,N), TiN and Al2O3, are frequently used in order to further enhance the performance of the cutting tool insert.

In the machining of steel (iron based metals) Al2O3 showing a high chemical and thermal stability, plays an important role acting as a diffusion barrier protecting the underlying cemented carbide from dissolution thus reducing the crater wear on the tool rake face. However, due to the sliding of work material against the rake face the relatively soft Al2O3 is exposed to both adhesive and abrasive wear which limits its lifetime in many cutting applications and consequently attempts have been made to improve the properties of CVD Al2O@3coatings, e.g. through the deposition of texture-controlled CVD Al2O3coatings.

The aim of the present study is to investigate the abrasive wear resistance of CVD Al2O3 coatings with different textures, i.e. <0112>, <1014> and <0001> and growth textures, using a micro-abrasion test with diamond particles as the abrasive medium. All CVD Al2O3coatings where deposited on cemented carbide substrates with an intermediate Ti(C,N) layer and the as-deposited coatings were characterised using X-ray diffraction and scanning electron microscopy. The results are discussed in relation to the results obtained from continuous turning tests using a quenched and tempered low alloyed steel, AISI 1045, and cast iron, AISI A48-45B, as work materials. The identified wear mechanisms of the coatings have been identified using scanning electron microscopy and energy dispersive X-ray spectroscopy. The potential of the micro-abrasion test in the tribological characterisation of thin CVD coatings for cutting tool applications is discussed.

3:50 PM B5-2-8 Low Temperature Alumina Coatings by AC Inverted Magnetron Sputtering Technique
A. Aryasomayajula, D. Bhat, M.H. Gordon (University of Arkansas); S. Singh, R. Kishore (National Physical Laboratory, India)
Crystalline alumina films were deposited on glass, silicon, stainless steel and carbide tool substrates using an inverted AC magnetron sputtering technique at 350°C. Two aluminum ring targets were used to sputter aluminum in an Ar/O2 plasma under different bias conditions. Some samples were pre-coated with an Cr2O3 template film prior to alumina deposition. The film structure was analyzed using XRD, SEM and EDAX. AFM was used for roughness measurement. Hardness was measured using a nanoindentation technique. The thickness of the films was measured using a ball and crater method. TEM was used for micro structural and phase analysis of alumina films. For TEM analysis 80-100 nm thin alumina films were deposited on carbon coated nickel TEM grids. The TEM analysis of these films showed a crystalline microstructure with a dominant Al2O3 (Corundum) phase. Initial machining tests were performed on the turning tools. In this paper, we will discuss our recent findings, and the data will be compared with the previously reported results by other workers. Keywords: AC magnetron sputtering, alpha alumina, characterization, machining.
4:10 PM B5-2-9 Characterization of DLC Coatings Deposited by Large Area Filtered Arc Deposition Technique
V. Gorokhovsky, Y.H. Cheng, C. Bowman (Arcomac Surface Engineering, LLC); A.A. Voevodin, C. Hunter (Air Force Research Laboratory); C. Muratore, Y. Kang (UTC Corporation); J.J. Hu (Montana State University); R. Smith, H. Chen, W. Priyantha (UTC Corporation)
The filtered arc coating deposition process is known as one which can deposit DLC coatings with the highest density, refractive index, hardness, low friction, low wear rate, high corrosion resistance and excellent biocompatibility, which enables a wide variety of applications in the microelectronic, data storage, optical, mechanical, aerospace, and biomedical industries. Using large area filtered arc deposition (LAFAD) dual arc sources alone or in combination with other PVD sources (unbalanced magnetrons, e-beam evaporators) it is possible to further modify structure and add additional elements into the coating. For all the applications, deposition of DLC coatings on different substrates with good adhesion is crucial. In this study, the LAFAD technique or hybrid LAFAD+UBM processes were used to deposit high quality DLC and doped DLC coatings. The influence of the DLC coating thickness, substrate material and substrate surface roughness, as well as the doping elements on the structure and adhesion of the DLC coatings were systematically studied by using various surface evaluation techniques. The interface microstructure and bonding structure between the DLC coatings and different substrates was investigated by using cross sectional TEM and XPS in addition to RBS technique. The carbon penetration into the substrate due to ion bombardment during DLC coating deposition process on carbide forming substrates, such as Ti, Si, Cr, and Fe was compared with the carbon distribution on a non-carbide forming Cu substrate. Cross sectional TEM and depth profile XPS results clearly show the formation of a carbide interface between the DLC coatings and carbide forming substrate. The formation of a carbon rich interlayer between DLC coatings and the different substrates correlates with the adhesion properties.
4:30 PM B5-2-10 Effect of Humidity on Lubricated Fullerene-Like Carbon Nitride Overcoats
E. Broitman, V.V. Pushkarev, A. Gellman (Carnegie Mellon University); A. Furlan, N.T. Son, L. Hultman (Linköping University, Sweden)
Humidity influences the tribological performance of the head-disk interface in magnetic data storage devices. In this work we compare the uptake of water of amorphous hydrogenated carbon and amorphous carbon nitride films, widely used as protective overcoats in computer disk drive systems, with fullerene-like carbon nitride films. Carbon films were deposited on quartz crystal substrates by reactive DC magnetron sputtering from a single isostaticaly pressed graphite target. Films were sputtered in an Ar/N2 atmosphere of 3 mTorr, N2 partial pressure between 16 % and 100 %, constant discharge current of 400 mA, and substrate temperature between 150 C and 450 C. After deposition, some of the films were coated with a 2 nm thick layer of Z-tetraol, a lubricant used in hard disk devices. A quartz crystal microbalance placed in a vacuum chamber was used to measure the adsorption of water at temperatures between 20 and 80 C, and pressures of water corresponding to relative humidities in the range RH = 0 to 90 %. Water adsorption and desorption is fast, indicating that equilibrium with ambient humidity is reached on timescales of minutes, much faster than the timescales for fluctuations in ambient humidity. Measurements indicate the amount of water adsorbed by the amorphous films is significantly higher than the fullerene-like ones. Electron microscopy and electron paramagnetic resonance have been used to correlate water adsorption to film microstructure and surface defects (dangling bonds).
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