TEM investigation of TiAlN/CrN multilayer coatings prepared
by magnetron sputtering
M. Panjan
⁎
, S. Šturm, P. Panjan, M. Čekada
Jožef Stefan Institute, Jamova 39, SI-1000 Ljubljana, Slovenia
Available online 2 June 2007
Abstract
Multilayer coatings TiAlN/CrN were deposited by reactive magnetron sputtering. Thickness of the individual layers varied from 2 nm to 25 nm
while the total thickness of the coating was ∼ 5 μm. Coatings in cross-section were investigated using conventional, scanning and high-resolution
transmission electron microscopy (TEM). Conventional TEM studies revealed a columnar microstructure. Chemical analysis of individual layers
was preformed by high-angle annular dark-field scanning TEM (HAADF-STEM). The layers were well separated and no substantial intermixing
was observed. High resolution TEM and electron diffraction studies showed that TiAlN and CrN layers are crystalline with B1 NaCl-type crystal
structure. Coherent interfaces between TiAlN/CrN were observed, which can be attributed to a small mismatch between lattice parameters. In
some areas between steel substrate (bcc-Fe) and the coating epitaxial relationship {001}
Fe
||{001}
coating
and b100N
Fe
||b110N
coating
was observed. In
different areas of the coating TiAlN layers appeared to be less crystalline than CrN.
© 2007 Elsevier B.V. All rights reserved.
Keywords: TiAlN/CrN; Multilayer; Magnetron sputtering; TEM; STEM; HRTEM
1. Introduction
Combination of different materials in a form of multilayers
produces coatings with superior properties than in the form of a
single layer. Especially good properties are found for nitride
materials with a few nanometer thick layers. These multilayers,
also termed superlattices, exhibit higher hardness, better
toughness, wear and oxidation resistance than constituent
materials deposited in a single layer. In the past years a variety
of different nitride multilayer coatings have been produced, for
example: TiN/CrN [1,2], TiN/NbN [3,4], AlN/VN [5], TiAlN/
CrN [6,7]. All of these coatings reach maximum hardness in a
narrow range of bilayer thickness of ∼ 3–10 nm. The maximum
hardness is always significantly higher than the hardness of the
materials in each layer. Several explanations have been
proposed for the origin of this effect including dislocation
blocking by layer interfaces, Hall–Petch strengthening, strain
effects at layer interfaces, and the supermodulus effect [8].
One of the most studied materials in the hard coating
technology are TiAlN and CrN. Properties of TiAlN depend on
the content of aluminum [9]. At the approximate 1:1 ratio of
titanium and aluminum atoms it is possible to get hardness higher
than 30 GPa [10]. TiAlN has very good oxidation resistance
compared to TiN [6]. CrN has lower hardness (∼ 18 GPa) but it is
tougher and thermally more stable [11]. Combination of these two
materials therefore yields a coating with good mechanical, wear
and oxidation properties [6,12]. The maximum hardness of
TiAlN/CrN superlattice was shown to be about 39 GPa for a
bilayer period of 6 nm [6].
Our aim was to investigate microstructure, crystal structure
and interfaces of TiAlN/CrN coating using cross-sectional
transmission electron microscopy (TEM). TEM is the only
technique with sufficient spatial resolution to resolve nanometer-
size layers in superlattices. Conventional TEM gives us detailed
information on microstructure, including grain size, orientation
and texture as well as on the types and distribution of defects
(dislocations, stacking faults). On the other hand, high-resolution
TEM (HRTEM) offers information on atomic scale with pos-
sibility to locally determine crystal structure and to study interface
characteristics (coherency, morphology, epitaxial relationships
between the layers). In spite of an immense number of papers
published on PVD coatings TEM investigations of such structures
are still relatively rare and detailed structure of PVD coatings on
Available online at www.sciencedirect.com
Surface & Coatings Technology 202 (2007) 815 – 819
www.elsevier.com/locate/surfcoat
⁎
Corresponding author. Tel.: + 386 1 477 3276; fax: +386 1 251 9385.
E-mail address: matjaz.panjan@ijs.si (M. Panjan).
0257-8972/$ - see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2007.05.084