TF4:
Mechanical Properties and Stress
Posters
TF4.1.P
INTERFACIAL ALLOYING INDUCED SHEAR ELASTIC
SOFTENING IN (111)Ni/(110)Mo MULTILAYERS
F. Martin1, G. Abadias*,1, J. Pacaud1, A. Debelle1, A. Michel1, C. Jaouen1,
Ph. Djemia2, F. Ganot2,
1
Laboratoire de Métallurgie Physique, UMR CNRS 6630, Université de Poitiers, SP2MI,
Téléport 2, BP 30179, 86962 Futuroscope-Chasseneuil cedex, France
2
Laboratoire des Propriétés Mécaniques et Thermodynamiques des Matériaux, UPR CNRS
9001, Université Paris Nord, Av. J. B. Clément, 93430 Villetaneuse cedex, France
The presence in some multilayers systems of deviations in the elastic behaviour
compared with that predicted by the continuum elasticity, so-called elastic "anomalies", has
given rise to the development of both considerable experimental and theoretical studies in
the past ten years, in order to determine the underlying mechanisms responsible for the
physical anomalies. The importance of the interfaces has long been recognized, although
their intrinsic nature (dilatation strains, structural disorder,...) is still subject to controversy.
The present study deals with the Ni/Mo system for which the elastic anomaly is one of
the most pronounced among those of the metallic binary systems reported in the literature
[1]. By combining X-ray Diffraction (XRD) and Brillouin light scattering (BLS)
experiments on both Ni/Mo superlattices and Ni1-xMox solid solutions samples, we show
that the formation of metastable alloys, obtained either by co-sputtering or stabilized at the
interfaces, induces an elastic lattice instability [2].
Ni/Mo multilayers with bilayer periods () ranging from 1.6 to 100 nm and Ni1-xMox
solid solutions samples were deposited on Si substrates using a high vacuum sputtering
apparatus system. Additional Ni/Mo samples were grown on monocrystalline saphire
susbtrates to investigate the epitaxial relationship and stress/strain states of both lattices.
For the Ni/Mo superlattices, a huge softening in the shear elastic constant (C44)
measured from BLS, is observed with decreasing . XRD experiments using the sin2
method show that the Mo layers are under high non-equal biaxial stresses, while the Ni
layers appear almost relaxed. In addition, the variation of the "stress-free" lattice parameter
of the Mo and Ni layers with suggest the presence of alloyed layers. For the solid
solutions, a drastic decrease in C44 is observed in the region where crystalline metastable
alloys are formed, while in the amorphous region, C44 no longer evolves. The stabilization
under epitaxial growth of supersatured interfacial alloyed layers into a crystalline state
could explain the extremely low value of C44 observed for the superlattices at small .
The influence of the energy of the sputtered atoms and growth rate on the residual
stresses and interfacial alloying was also studied for Ni/Mo superlattices with =7.5 nm.
[1] I.K. Schuller, A. Fartash, M. Grimsditch, MRS Bulletin, vol.15 (10), 33, 1990
[2] G. Abadias, C. Jaouen, F. Martin et al., Phys. Rev. B, submitted
*Corresponding author : Tel : +33 5 49 49 67 48, Fax : +33 5 49 49 66 92
e-mail : gregory.abadias@univ-poitiers.fr
TF4.2.P
THE INFLUENCE OF MECHANICAL ADHESION OF COPPER
COATINGS ON CARBON SURFACES ON THE INTERFACIAL
THERMAL CONTACT RESISTANCE
E.Neubauer1/2, G. Korb1, C.Eisenmenger-Sittner2, H.Bangert2
S.Chotikaprakhan3, D.Dietzel3, A.M.Mansanares3, B.K.Bein3
*
ARC Seibersdorf Research GmbH, Dept. Materials and Production Engineering
Vienna University of Technology, Institute of Solid State Physics - Thin Film Group
***
Ruhr Universität Bochum, Exp.Phys.III, Solid State Spectroscopy Group
**
Metal matrix composites based on copper reinforced with carbon fibers are expected to
have a high thermal conductivity and a low Coefficient of Thermal Expansion (CTE).
Nevertheless due to a weak interface between copper and carbon fibers which is related to
the absence of any reactivity or dissolution between the constitutents, a „thermal gap“ at the
interface limits the use of this material for thermal management applications.
In order to optimise the thermal as well as the mechanical interface of this material combination, investigations were started on a simplified plane model system, consisting of a
copper coating deposited by PVD on a glassy carbon surface. Starting with different
cleaning procedures of the substrate, the influence on the mechanical adhesion strength of
the copper coating was investigated by a pull-off method. In addition to the surface treatment, the influence of an intermediate layer on the adhesion strength was investigated.
Parallel to the investigation of the adhesion strength, the thermal contact resistance at the
interface was determined using a photothermal method of characterisation, which is based
on modulated Argon ion laser beam heating of the coating, leading to periodical thermal
waves which propagate across the coating and the interface. At the interface reflection
occurs, and from the amplitude and phase shift of the thermal wave response, measured by
contactless IR radiometry at the surface of the heated coating, a quantitative description of
the interfacial thermal resistance is obtained. It was shown that this method is a suitable
tool to characterise thermal interfaces of 1µm copper layers on a glassy carbon surface
having different mechanical adhesion strength. A good correlation between the thermal and
mechanical interface was found.

Corresponding author: Tel.:+43-50-550-3345; Fax.:+43-50-550-3345. E-mail: erich.neubauer@arcs.ac.at
TF4.3.P
CORRELATION BETWEEN WEAR RESISTANCE AND
MECHANICAL PROPERTIES FOR Ge-As(Sb)-S(Se) THIN FILMS
Nicolai D. Savchenko
Uzhgorod National University, Ukraine
Thin films obtained from the chalcogenide glasses have found commercial application
in infrared optics, opto- and microelectronics [1]. The prospects of their use for the
protective, passivating and optical coatings have been discussed in a number of works. An
information on the wear resistance is of great interest for the design of the coatings based
on these materials. In this work the attempt to determine the empirical relationships
between the comparative wear resistance of some chalcogenide Ge-As(Sb)-S(Se) films and
their physical and mechanical properties has been made.
The Young’s modulus, microhardness, linear thermal expansion coefficient, stress, fow
limit, adhesion and shear strength for As2S3, As2Se3, Ge28Sb12Se60, Ge33As12Se55,
Ge36As4S60 films obtained by thermal evaporation in vacuum onto ZnSe substrates have
been measured. The calculations of the molar fractions for chemical bonds, molar
volume (), average bond breaking energy (Ebb) for the glasses under investigation have
been conducted.
The measurements of the wear resistance have been carried out by the device described
in [2]. In this device the samples are rubbed by the application of a force of about
(2.00  0.01) N to the film via the rubbing tip at a distance of ro = 5  10-3 m from the
rotational axis of the sample rotating at an angular speed of 500 RPM. Thin films were
rubbed by the batiste cloth moving at a speed of 5.0  10-4 m/s. The wear products have
been removed from the zone of friction and a number of revolutions stood by the sample up
to the moment when the scratch cuts through the film has been determined. To determine
the comparative wear resistance for the films the experimental data have been rated to the
wear resistance of Ge16Sb24Se60 film taken for a unit. Wear resistance has been determined
with the accuracy better than 3 %. The coefficient of variation was about  7 %.
The mechanical parameters of thin films have been measured following the
experimental procedure given in [3]. The interrelationships between the mechanical
properties of thin films under investigation has been analysed. The empirical equations
relating the comparative wear resistance to adhesion strength, Young’s modulus and
microhardness have been derived. Correlation between the comparative wear resistance
and Ebb/ value has been revealed. The effect of the additional stress arising from the
temperature increase under the work done by fictional forces on the comparative wear
resistance has been shown.
[1] Proc. of the First Intern. Workshop on Amorphous and Nanostructured Chalcogenides Fundamentals and Applications (ANC-1), Part I, Bucharest , Romania, June 25-28,
2001. Journal of Optoelectronics and Advanced Materials, 2001, vol. 3, No.2, 583 p.
[2] A. G. Anchugin, N. D. Savchenko, G. S. Salishchev, M. A. Shakhaida, Yu. Yu. Firtsak,
Patent USSR No. 1528121, dated 08. 08. 1989.
[3] T. N. Shchurova, N. D. Savchenko. Journal of Optoelectronics and Advanced
Materials, 2001, Vol. 3, No. 2, p. 491 - 498.
Corresponding author: Nicolai D. Savchenko
Uzhgorod National University, Department of Engineering
13 Kapitulna St., Uzhgorod 88000, Ukraine
Tel./fax: +038 03122 30656
e-mail: root@tv.uzhgorod.ua
TF4.4.P
DEPOSITION FACTORS EFFECT ON THE MECHANICAL
STRENGTH FOR Ge30As4S66 THIN FILMS
T. N. Shchurova, N. D. Savchenko, M. L. Trunov
Uzhgorod National University, Ukraine
Thin films obtained by thermal evaporation of Ge30As4S66 glasses have been reported to
be used for the preparation of the different types of the interference coatings for near and
middle infrared [1]. Information on the mechanical properties, e.g. Young’s modulus,
microhardness, adhesion and shear strengths, stress, should be taken into account in the
process of the design of the coating or other film structure. It is known that these
mechanical parameters depend on the following conditions of film deposition process:
substrate temperature, deposition rate, residual pressure, etc., as well as on the subsequent
film processing, e.g. thermal or laser treatment, irradiation and so on. Earlier [2] we have
studied the mechanical properties of Ge30As4S66 thin films deposited in vacuum at pressure
of 10-4 Pa onto ZnSe substrates at deposition rate of 6.0 nm/s. In this work the results of the
investigation of the effect of deposition rate (2 - 18 nm/s) and substrate temperature (300 375 K) on stress, adhesion and shear strengths for amorphous Ge30As4S66 films have been
presented along with the effect of thermal (450 K for 1 hour) and laser (W = 0.2 Wt/cm2,
 = 0.514 m) treatment on the Young’s modulus, linear thermal expansion
coefficient (LTEC), microhardness, stress, fow limit, adhesion and shear strength. The
experimental details on samples preparation and measurement of thin film mechanical
parameters is given in [2].
To determine the correlation between adhesion and shear strength and between adhesion
strength and stress the studies have been performed on the films deposited onto the
substrates with different LTEC (BaF2, SiO2, Ge, GaAs, Si) heated to the same temperature.
For the adhesion (a) and shear (sh) strength the relation a = 0.2к has been found. The
relationship а = (1.2  106 + 0,025 ) Pa has been derived between the adhesion strength
and stress () for stress values below the flow limit, when for the ones above this limit the
found relation was а = (6.7  106 + 0,170 ) Pa.
It has been shown that the observed features of the substrate temperature and deposition
rate effect on the adhesion and shear strength of thin films under investigation were related
to the elastic deformation of the film.
[1] Optics in Ukraine. Science and Production Guide / SPIE - The International Society for
Optical Engineering, Ukrainian Chapter. Kyiv, 1996, p. 134-146.
[2] T. N. Shchurova, N. D. Savchenko. Journal of Optoelectronics and Advanced
Materials, 2001, Vol. 3, No. 2, p. 491 - 498.
Corresponding author: Tatiana N. Shchurova, Uzhgorod National University, Department
of Engineering 13 Kapitulna St., Uzhgorod 88000, Ukraine, Tel./fax: +038 03122 30656
e-mail: taina@tv.uzhgorod.ua
TF4.5.P
LATTICE AND MICRO-STRAINS IN POLYCRYSTALLINE SILICON
FILMS DEPOSITED ON CERAMIC SUBSTRATES
P. Šutta(1) and Q. Jackuliak(2)
Department of Physics, Faculty of Logistics, Military Academy,
O31 19 Liptovský Mikuláš, Slovakia
(2)
Dept. of Tech. Phys., Faculty of Electrical Engineering, University of Žilina,
010 26 Žilina, Slovakia
E-mail: sutta@valm.sk; qjackk@fel.utc.sk
(1)
Polycrystalline silicon thin films are considered to be a promising candidate for lowcost photovoltaic application [1]. In order to obtain the low-cost production and good
quality of films, an appropriate technology and substrate have to be choosen. Novel
ceramic materials as mullite and SiAlONs and alumina as a typical conventional substrate
could be suitable for the silicon deposition using a thermal CVD process. Silicon thin films
10 m in thickness were deposited onto the three different substrates: SiAlON, mullite and
alumina by using a thermal CVD method within the deposition temperature range between
900o C to 1100o C [2]. In order to achieve the optimal photovoltaic conversion efficiency,
the material has to possess the minority carrier diffusion length and mean minority carrier
life time as much as possible. In a polycrystalline thin film these characteristics strongly
depend on microstructure of the material used. Lattice (macro-) stress, microstress,
crystallite size, prefered orientation of crystallities (texture) and stacking faults belong to
the most important structure properties of polycrystalline films deposited on substrates.
These main structure properties of films strongly depend not only on the deposition
conditions but also on a microstructure of a substrate used in particular when the substrate
is polycrystalline.
In this paper, the microstructure characterization of silicon films was carried out by
means of X-ray diffraction analysis on a common X-ray powder diffractometer with a
Bragg-Brentano goniometer. Size-strain analysis was performed by using X-ray diffraction
line profile analysis of five the most intensive silicon diffraction lines and preferred
orientation of crystallities was evaluated according to a Harris texture index. The lattice
stress was obtained from a shift of the silicon diffraction lines against to strain free
reference positions of lines calculated from theory for the total randomly oriented grains of
the film. X-ray diffraction analysis indicated that the all silicon films are polycrystalline.
The preferred orientation of silicon films deposited on SiAlON is almost in [110] direction
perpendicular to the substrate, whereas the preferred orientation of the silicon films
deposited on mullite and alumina is in [111] direction. The crystallite sizes reach from
several hundreds of nanometers in Si films on mullite and alumina to several micrometers
in Si films on SiAlON depending on deposition temperature and crystallographic
orientation (h k l). The tensile lattice stress decreasing with increasing deposition
temperature was observed in Si films on SiAlON, whereas the compressive lattice stress
was observed in Si films deposited on mullite and alumina substrates. The probability of
stacking faults of 0.005 was observed only in direction [110] in Si film on alumina
deposited at 1100o C. In the other silicon films were stacking faults not observed at all.
[1]A.J.M.M. van Zutphen, P. Šutta, F.D. Tichelaar, A. von Keitz, M. Zeman, J.W.
Metselaar, Journal of Crystal Growth 223 (2001) pp. 332-340.
[2] A.J.M.M. van Zutphen, PhD. thesis, Delft University of Technology, 2001.
TF4.6.P
LOW-ENERGY ION MODIFICATION
OF TiN FILMS
TARASENKO Y.P., TSAREVA I.N., ROMANOV I.G., MYSHLYAYEV D.A.
Nizhny Novgorod Branch of
Mechanical Engineering Research Institute, RAS.
603024, Nizhny Novgorod, Belinskogo, 85, Russia.
The TiN films are widely used in the industry. But the development of new technique
needs more details investigation of structural parameters of such material and futher
modification of its mechanical and tribological properties. The properties of TiN films
produced by ion-plasma method under 0,2-0,8 Pa before and after to low energy ( 1 keV)
irradiation Ti
+
ion beams are presented. Electron microscopy analysis showed increasing
or decreasing of microdeformation, bloch size and dislocation density for different time of
ion treatment. Those structural changes by affected microhardness and coefficient of
friction. The results of friction properties study are discussed within the framework of the
andhesional-deformation theory.