Journal of the European Ceramic Society 36 (2016) 3059–3066
Contents lists available at www.sciencedirect.com
Journal of the European Ceramic Society
jo ur nal home p ag e: www. elsevier.com/locate/jeurceramsoc
Nanoindentation induced deformation anisotropy in -Si
3
N
4
ceramic
crystals
Tamás Csanádi
a,∗
, Duˇ san Németh
a
, Ján Dusza
a,b
, Zoltán Lenˇ céˇ s
c
, Pavol
ˇ
Sajgalík
c
a
Institute of Materials Research, Slovak Academy of Sciences, Watsonova 47, 04353 Koˇ sice, Slovak Republic
b
Donát Bánki Faculty of Mechanical and Safety Engineering, Óbuda University, Népszínház utca 8, 1081 Budapest, Hungary
c
Institute of Inorganic Chemistry, Slovak Academy of Sciences, Dúbravská cesta 9, 845 36 Bratislava, Slovak Republic
a r t i c l e i n f o
Article history:
Received 30 July 2015
Received in revised form
13 November 2015
Accepted 24 November 2015
Available online 11 December 2015
Keywords:
-Si3N4
Indentation modulus
Nanohardness
EBSD
Anisotropy
a b s t r a c t
The influence of crystal orientation on nanohardness and indentation modulus of grains in polycrystalline
-Si
3
N
4
was studied under nanoindentation at room temperature. The orientation of the individual grains
was determined by electron backscatter diffraction (EBSD) prior to the indentation. Significant elastic and
plastic deformation anisotropy was revealed. The elastic modulus exhibited a decrease for grains oriented
from the basal towards the prismatic facets while the nanohardness values showed reversed tendency.
The orientation dependence of indentation modulus was predicted by the Vlassak-Nix model and finite
element model (FEM) calculations based on the elastic constants of -Si
3
N
4
single crystal and compared
to the experimental results. A theoretical model was proposed to describe the nanohardness anisotropy
on the basis of the possible slip systems of -Si
3
N
4
. The calculations for elastic and plastic anisotropy are
in good agreement with the experimental results.
© 2015 Elsevier Ltd. All rights reserved.
1. Introduction
For more than fifty years, silicon nitrite based ceramics are still
one of those advanced materials which are in the centre of interest
owing to their attractive mechanical properties, such as high hard-
ness, strength and wear resistance. These properties are attributed
mostly to the high energy covalent bonds which make silicon nitrite
possible for wide range of applications such as cutting tools, ball
bearings or heat engine parts [1]. Silicon nitride exists in two major
crystallographic modifications, and . Both have hexagonal struc-
ture and -Si
3
N
4
(space group P6
3
/m) is the more stable one due
to the → phase transformation which occurs at higher temper-
atures [1,2].
It is well known that the mechanical and fracture properties
of bulk polycrystalline silicon nitride ceramics are strongly influ-
enced by the properties of the individual grains and intergranular
phases, as well as by the structure of interface between the grains
and intergranular phases [3–5]. Therefore, in order to design opti-
mized microstructure with enhanced combinations of hardness,
toughness and wear resistance, it is important to understand the
∗
Corresponding author.
E-mail address: tcsanadi@imr.saske.sk (T. Csanádi).
anisotropic deformation behaviour of the individual -Si
3
N
4
crys-
tals.
Plasticity of macroscopically brittle materials, focusing here
only on silicon nitride
,
is commonly investigated by means of
micro-, nanoindentation testing and more recently by micropil-
lar compression [6–14]. Table 1 gives a summary of the results of
the most relevant studies which aimed to characterize the effect
of crystallographic orientation of -Si
3
N
4
single crystal grains on
their hardness.
One of the first attempts to characterize the deformation
behaviour and the hardness anisotropy of Si
3
N
4
single crystals were
performed by Chakrabotry and Mukerji [6] and Reimanis et al. [7].
They investigated the microhardness of differently oriented crys-
tallographic planes in - and -Si
3
N
4
single crystals and reported
higher hardness values corresponding to the prismatic plane com-
pared to basal facet. Later, similar hardness anisotropy was revealed
by Dusza et al. [8,9] in -Si
3
N
4
grains of gas pressure sintered poly-
crystalline Si
3
N
4
founding also significantly higher hardness values
belonging to the prismatic plane than that on the basal one. It is
important to emphasize that these investigations are focused on
the two extreme crystal orientations, namely on the basal and the
prismatic orientations. Up to now, the only relevant paper which
attempted to map the general orientation dependence between the
basal and the prismatic orientations is the nanoindentation study
of Hay et al. [10]. In their work, the influence of crystal orienta-
http://dx.doi.org/10.1016/j.jeurceramsoc.2015.11.028
0955-2219/© 2015 Elsevier Ltd. All rights reserved.