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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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of AISI 52100 steels by developing the powder-pack boriding method. The<br />

treatment was carried out at a temperature of 1223 K with 1 h of exposure.<br />

The boriding of AISI 52100 steels results in the formation of a superficial<br />

flat front growth of FeB/Fe2B layers with a total layer thickness of 72<br />

microns. In addition, the hardness at the surface of borided steels was 1900<br />

HV.<br />

The four-ball lubricant tests were performed in the borided samples (with a<br />

surface roughness of 0.043 microns) and unborided steels with a surface<br />

roughness of 0.025 microns considering dry and lubricant conditions. The<br />

wear resistance of borided and unborided steels in the dry condition was<br />

estimated by three different loads of 49, 98 and 147 N with a constant speed<br />

and time test of 1200 rpm and 150 s, respectively. For the case of the<br />

lubricated condition, the borided and non-borided steels were exposed to<br />

applied loads of 147 and 392 N according to the ASTM D4172 standard<br />

using commercial SAE 15W40 engine oil. For all cases, the friction<br />

coefficients of borided and unborided steels were monitoring by a full<br />

bridge load cell, and the temperature was sensed through a thermocouple in<br />

real time during the four-ball lubricant test. The wear scar diameter and the<br />

wear scar surfaces of the AISI 52100 borided and non-borided steels in both<br />

experimental conditions were measured using an optical microscope and<br />

scanning electron microscopy (SEM) to understand the wear mechanisms<br />

involved.<br />

Considering the dry condition, the results of the friction coefficient showed<br />

that the presence of boride layers at the surface of AISI 52100 steels denote<br />

solid lubricating features, where this characteristic is increased in lubricant<br />

conditions as a function of the different applied loads.<br />

New Horizons in <strong>Coating</strong>s and Thin Films<br />

Room: Sunset - Session F2-1<br />

High Power Impulse Magnetron Sputtering<br />

Moderator: D. Lundin, Université Paris-Sud 11, France, J.<br />

Sapieha, Ecole Polytechnique de Montreal, Canada, R.<br />

Bandorf, Fraunhofer Institute for Surface Engineering and<br />

Thin Films IST, Germany<br />

8:00am F2-1-1 Energetic aspects of thin film growth in HiPIMS and in<br />

other pulsed plasmas, L. Martinu (lmartinu@polymtl.ca), J. Capek, M.<br />

Hala, O. Zabeida, J.E. Klemberg-Sapieha, École Polytechnique de<br />

Montréal, Canada INVITED<br />

The microstructure and the resulting properties of coatings and thin films<br />

strongly depend on the growth mechanism which in turn is closely related<br />

to the energetic aspects of surface reactions during the material’s synthesis.<br />

It has been accepted that the microstructural evolution of films grown in<br />

ionized and plasma environments can be well described in terms of the ion<br />

energy and ion flux, or specifically, in terms of the “universal parameter:<br />

the energy per deposited atom”.<br />

Film growth, while under ion bombardment, leads to growth-related effects<br />

such as interfacial atom mixing, high surface mobility (diffusion) of<br />

deposited species, resputtering of loosely bound species, and deep<br />

penetration of ions below the surface, leading to the displacement of atoms<br />

(forward sputtering or knock-in effects). The energy and flux of ions can<br />

generally be controlled, to different levels of selectivity, by the use of ion<br />

beams, by surface biasing, and by the control of plasma density. Compared<br />

to more traditional PECVD and PVD techniques (including DC, pulsed DC,<br />

and medium-, radio- and microwave frequency discharges), there has been a<br />

lot of progress in generating very dense plasmas in pulsed discharges, more<br />

recently in High Power Impulse Magnetron Sputtering (HiPIMS). The latter<br />

technique offers a unique possibility to obtain films from a high flux of<br />

highly ionized materials.<br />

In this presentation, we will critically evaluate the energetic aspects of the<br />

film growth in HiPIMS plasmas, and compare the resulting film<br />

characteristics with those obtained by other techniques. Examples will<br />

include hard protective coatings (conductive or partially conductive), as<br />

well as optical (generally non-conductive) coatings. We will review<br />

different strategies for the control of the deposition process, and discuss<br />

various effects related to the pulse management, to the suppressions of<br />

hysteresis, and to the magnetic field configuration at the target surface.<br />

8:40am F2-1-3 Unique Property of Our Brand New Technology Based<br />

On High Power Pulse Sputtering., S. Hirota<br />

(hirota.satoshi@kobelco.com), K. Yamamoto, Kobe Steel Ltd., Japan, R.<br />

Cremer, KCS Europe GmbH, Germany<br />

We introduce a brand new technology based on High Power Pulse<br />

Sputtering at industrial scale. The New Technology is a magnetron<br />

discharge process like conventional sputtering, however, momentarily input<br />

power is approximately ten times higher in magnitude. Conventional<br />

magnetron sputtering is a low current - high voltage discharge and the<br />

ionization rate of the target material is quite low, usually in the order of a<br />

few percent and the plasma is mainly consisting of gas ions. On the other<br />

hand the New Technology realized stable operation with high current - high<br />

voltage discharge with high ionization rate of the target material and high<br />

deposition rate compared to conventional sputtering. This unique property<br />

is characterized by controlling pulse shape of input power, this means the<br />

film property generated by the New Technology can be modified with great<br />

flexibility.<br />

In this study, we analyzed film property by changing coating condition and<br />

compared with another coating process. For example, different types of<br />

nitride coatings including standard TiAlN were deposited by industrial arc<br />

ion plating (AIP), unbalanced magnetron sputtering(UBMS) and New<br />

Technology . TiAlN coatings deposited by the New Technology process<br />

show strong preferred (111) orientation and a relatively high hardness up to<br />

35 GPa. Whereas AIP TiAlN coatings are characterized by a moderate<br />

hardness up to 30 GPa and (200) or nearly random orientation at an<br />

equivalent substrate bias condition. High magnification image of cross<br />

sectional TEM observations of both coatings revealed that many lattice<br />

defects can be observed for the New Technology coating and is hardened by<br />

many atomic defects, possibly highly stressed as a consequence.<br />

In the presentation, a comparison between AIP, UBMS and the New<br />

Technology coating by different power supply, arc source and deposition<br />

conditions will be shown, not only from property of the coating but also<br />

from industrial perspective such as productivity.<br />

9:00am F2-1-4 Influence of pulse shape and peak current on the<br />

resulting properties of Ti-Si-C composite films deposited by HIPIMS,<br />

R. Bandorf (ralf.bandorf@ist.fraunhofer.de), M. Scholtalbers, G. Bräuer,<br />

Fraunhofer IST, Germany<br />

In recent years the interest in ternary systems, especially so called Mn+1AXn<br />

phases has grown. This interest is motivated by the exceptional structural,<br />

electrical, and mechanical properties of these materials. Besides several<br />

investigations of DC sputtered Ti3SiC2 Alami et al. reported on HIPIMS<br />

deposition. The film structure was reported being columnar, both in dc and<br />

HIPIMS. While the HIPIMS films obtained a dense structure, the dc films<br />

were rough and porous. This paper shows that with HIPIMS deposition<br />

even a featureless glassy structure can be realized, depending on the<br />

deposition parameters. XRR measurements showed that by using HIPIMS<br />

with target current density of approx. 0.5 A/cm 2 a film density of 4.5 g/cm 3 ,<br />

correlating with the bulk value was reached. Furthermore, the resulting<br />

structure and properties (electrical and mechanical) depending on the used<br />

pulse shape during deposition are discussed.<br />

9:20am F2-1-5 Highly ionized carbon plasmas for the growth of<br />

diamond-like carbon thin films with magnetron sputtering, A. Aijaz, K.<br />

Sarakinos, D. Lundin, U. Helmersson (ulfhe@ifm.liu.se), Linköping<br />

University, Sweden<br />

The physical vapor deposition methods, characterized by highly ionized<br />

deposition fluxes of the film forming species, provide added means for the<br />

synthesis of tailor-made materials. Cathodic arc and pulsed laser deposition<br />

are examples of such discharges where electron densities in the order of<br />

10 21 m -3 can be obtained. These techniques, while providing a very high<br />

degree of ionization of the deposition flux, often exhibit several drawbacks,<br />

such as macroparticle ejection from the target, lack of lateral film<br />

uniformity, and difficulty to scale up. Magnetron sputtering based<br />

techniques are technologically interesting, owing to their inherent<br />

advantages of conceptual simplicity, scalability, and film uniformity.<br />

However, electron densities in magnetron discharges are significantly<br />

smaller, in the range of 10 14 -10 16 m -3 and therefore generation of a highly<br />

ionized deposition flux is often difficult. This difficulty is overcome by high<br />

power impulse magnetron sputtering (HiPIMS), where plasma densities on<br />

the order of 10 19 m -3 are achieved. HiPIMS has been successful in<br />

enhancing the ionization for most common metals (Cu, Al, Ta, Ti), but it is<br />

challenged by C. Previous investigations have shown that C + /C ratio in<br />

HiPIMS does not exceed 5% [1]. In the present study we address the low<br />

degree of C ionization by increasing the electron temperature of the plasma.<br />

This is achieved in the HiPIMS discharge by using Ne as sputtering gas<br />

instead of Ar. It resulted in an energetic C + ion population with a three-fold<br />

increase in the total number of C + ions as compared to a conventional<br />

HiPIMS process. The enhanced ionized fraction of carbon facilitates the<br />

growth of carbon films with mass densities as high as approx. 2.8 g/cm 3 as<br />

determined by high resolution x-ray reflectively measurements.<br />

[1] B.M. DeKoven, P.R. Ward, and R.E. Weiss, D.J. Christie, R.A. Scholl,<br />

W.D. Sproul, F. Tomasel, and A. Anders, Proceedings of the 46th Annual<br />

Technical Conference Proceedings of the Society of Vacuum Coaters, May<br />

3-8, 2003, San Francisco, CA, USA, vol., p.158<br />

35 Tuesday Morning, April 24, <strong>2012</strong>

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