Materials Science and Engineering A 442 (2006) 543–546

Automated resonant vibrating-reed analyzer apparatus for a non-destructive

characterization of materials for industrial applications
S. Amadori a , E.G. Campari a , A.L. Fiorini a,∗ , R. Montanari b , L. Pasquini a ,
L. Savini a , E. Bonetti a
a Dipartimento di Fisica, Università di Bologna, INFM and CNISM, V.le Berti Pichat 6/2, I-40127 Bologna, Italy
b Dipartimento di Ingegneria Meccanica, Università di Roma Tor Vergata, Via di Tor Vergata, I-00133 Roma, Italy
Received 29 July 2005; received in revised form 20 January 2006; accepted 6 February 2006

Abstract
A completely automated vibrating-reed apparatus for measurements of the mechanical quality factor and dynamic elasticity moduli has been
developed. The apparatus is equipped with heating and cooling stages allowing continuous temperature ramps and isothermal measurements in the
range 90–1400 K. Measurements in a magnetic field up to 8 × 104 A/m can also be performed. The data acquisition is computer-controlled through
a software specifically developed allowing, with a high acquisition rate, automatic measurements and control of all the apparatus components
and real-time data analysis. Some results are reported to illustrate the capabilities. These refer to bulk submicro-grained alloys obtained by severe
plastic deformation, nanocrystalline metal hydrides for hydrogen storage and metal foams. The results are briefly discussed to emphasize the utility
of employing mechanical spectroscopy in synergy with other techniques for a structural and functional characterization of various materials for
industrial applications.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Vibrating-reed analyzer; Submicro-grained alloys; Nano metal hydrides; Metal foams

1. Introduction mechanical quality factor, which is of relevance in defining some

It is well known that the elastic energy dissipation mech-
anisms in materials are directly connected to many differ-
ent physico-chemical processes, determining materials prop-
erties that are relevant for industrial applications. The anelas-
tic behaviour of materials is at the origin of the mechanical
energy dissipation and among the intrinsic sources of anelas-
ticity, including both relaxational and structural damping pro-
cesses, of paramount relevance are the short range dynamics of
structural defects, such as point defects, dislocations and inter-
faces and some phase transitions. The related micromechanisms
induce reversible or irreversible modifications in the structure-
sensitive properties and components of the elasticity moduli,
which cannot be regarded, strictly speaking, as materials con-
stants.
The elastic energy dissipation is characterized through the
dimensionless quantity, internal friction. It is the inverse of the
∗ Corresponding author. Tel.: +39 051 2095298; fax: +39 051 2095153.
E-mail address: annalisa.fiorini@bo.infm.it (A.L. Fiorini).
performance index, used for an efficient selection of materials,
when specific damping levels are required. Moreover, in res-
onant frequency techniques, the vibration frequency, which is
proportional to the relevant elastic constant of the material, is
another important parameter to evaluate modifications in the
elastic moduli induced by operating conditions.
Many apparatus generally referred to as mechanical analyz-
ers have been developed in recent years [1]. They span from
the classical torsion pendulum to those operating in free-free
or clamped-free geometries, in flexural vibrations. All these
apparatus are automated and employ generally user-friendly
interfaces allowing and promoting their use as standard char-
acterization tools in different areas of materials science and
industrial laboratories. Mechanical analyzers of the resonant
type offer generally better performances with respect to those
working in forced vibration because they allow a better sen-
sitivity; they and can be employed with materials with high
mechanical quality factor Q > 104 [2]. The aim of this paper is to
describe some applications of an automated resonant mechani-
cal analyzer recently developed in our laboratory to investigate
materials employed in various technological applications.

0921-5093/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2006.02.210
544 S. Amadori et al. / Materials Science and Engineering A 442 (2006) 543–546
Fig. 1. The block diagram of VRA-1604 apparatus.
2. Experimental
All measurements of the dynamic Young’s modulus and of
the internal friction coefficient have been performed by means
of the vibrating-reed analyzer VRA-1604,1 Fig. 1.
This analyzer has some specific facilities: it operates at
heating–cooling rates selectable in a wide range, under a high
vacuum (10−5 Pa) obtained with a turbomolecular pump. Con-
tinuous thermal runs as well as isothermal measurements in the
range 90–1400 K are possible. It is possible to perform mea-
surements in a varying magnetic field up to 8 × 104 A/m. The
program controlling the whole functions, data acquisition and
elaboration was developed with LabView software. It includes
a remote control of the function generator, power supply for the
oven and the coil generating the magnetic field. The measure-
ment procedure can be predetermined to operate simultaneously
during a run in different vibration modes, that is, different vibra-
tion frequencies in the accessible frequency range. Constant
strain or stress conditions can be selected. In this way measure-
ments at constant temperature as a function of strain amplitude
in the range 10−6 to 10−4 are also possible.
3. Anelasticity in aluminium alloys subjected to severe
plastic deformation
Sub-micron grained alloys prepared by severe plastic
deformation techniques, such as equal channel angular pressing
(ECAP) [3], have recently received much attention, owing to
their high strength near room temperature and their potential for
superplasticity at high strain rates. In the last years many alu-
minium alloys have been processed by ECAP. The Al–Mg–Si
ones are among the precipitation hardenable alloys mostly
investigated. In particular, of great technological interest is to
understand if a synergic effect of the different strengthening
1 VRA-1604 is a trademark of CANTIL SrL, Italy.
Fig. 2. Internal friction Q−1 and dynamic Young’s modulus E of: (a) alloys
as extruded (in the inset the high-temperature Young’s modulus trend in the
alloy with Sc addition) and (b) after ECAP starting from over-aged conditions.
The values of the dynamic modulus are normalized to those measured at room
temperature (E0 ).
mechanisms is operative: that is, if strengthening by grain
refinement through severe plastic deformation can join with
precipitation hardening. Investigations have recently been
performed by mechanical spectroscopy on a 6082 Al–Mg–Si
alloy supplied by Hydro-Norsk as extruded 10 mm diameters
cylindrical billets with chemical composition (in mass%):
0.34 Mg, 0.51 Si, 0.16 Fe, 0.014 Mn, 0.10 Zr, and a similar
alloy containing Sc: 0.33 Mg, 0.52 Si, 0.17 Fe, 0.014 Mn, 0.10
Zr, 0.117 Sc [4]. The anelasticity spectra in Fig. 2(a) and (b)
are a good example of the potential of this structure-sensitive
technique to monitor the microstructural evolution. The alloy
in the as extruded condition, Fig. 2(a), shows two prominent
features: a structural damping maximum, just preceding the
recrystallization, corresponding to a well evident increasing
step in the dynamic Young’s modulus. This process in the alloy
containing Sc occurs at higher temperatures. The anelastic
relaxation peak present at approximately 570 K (103 Hz) is well
resolved in the alloy without Sc addition, Fig. 2(a), while its
relaxation strength is strongly depressed in the Sc containing
alloy. This effect is attributed to dragging by Mg solutes, or
MgSi complexes, of dislocation loops pinned by precipitates [5].
The anelasticity spectra of the over-aged, ECA-pressed alloys
are reported in Fig. 2(b). A close inspection of the results with
reference to those reported in Fig. 2(a) allows to derive some
indications on the microstructure resulting from the severe plas-
tic deformation process and on its thermal stability. At room
temperature the damping is generally increased by a factor
 S. Amadori et al. / Materials Science and Engineering A 442 (2006) 543–546 545

two, and a strong increase with temperature is observed at A damping peak is observed at 590–600 K (103 Hz) in Fig. 3.
temperatures significantly lower (roughly 100 K) than in the Comparison of trends in successive thermal runs indicates
corresponding samples before ECAP. A maximum is reached strong irreversible reduction of the peak height and resonance
at approximately 490–510 K (samples without Sc) with a cor- frequency. The XRD spectra after the first thermal run show the
responding inverse trend in the modulus. These high damping presence of magnesium and only minor traces of magnesium
values at temperatures where appreciable grain growth in the hydride, indicating that significant hydrogen desorption has
submicro-crystalline ECA-pressed alloys is not expected are occurred.
consistent with transmission electron microscopy (TEM) and
scanning electron microscopy (SEM) observations [6], indicat-
5. Foamed aluminium
ing that a high fraction of non-equilibrium grain boundaries are
present. Grain growth is indeed observed at higher tempera-
In some classes of materials, damping properties are techno-
tures. This maximum should mark the upper-limit temperature
logically important, for example, when a high damping capacity
for the occurrence of the optimum conditions for superplastic
is required. Foamed materials and, specifically, metal foams
behaviour, and is associated with a transformation of the non-
have found potential for industrial applications when weight
equilibrated disordered high-angle grain boundaries into more
reduction or sound and energy absorption are a prerequisite.
ordered ones [6].
Mechanical spectroscopy may yield very useful pieces of infor-
mation on the elastic energy dissipation mechanisms in these
4. Nanocrystalline magnesium hydrides for hydrogen
materials. A question not completely solved yet is the reported
storage
high damping capacity of metallic foams and in general other
cellular metallic materials [9], and at the same time their strong
Metal hydrides have recently received increasing interest
amplitude-dependent damping [10]; a careful characterization
owing to their potential application as energy storage mate-
of the mechanical properties in the elastic–anelastic range, in
rials. Magnesium hydride, in particular, has a high hydrogen
dependence of various structural and processing parameters,
storage capacity (7.6 mass%) and a large formation enthalpy
is required for a full understanding of the mechanical prop-
(H = −75 kJ/mol). For technological applications, research
erties. Some preliminary measurements have been performed
efforts aim at overcoming some critical aspects and reach an
improvement of the reaction kinetics and, at the same time, a
reduction of the desorption temperature. A significant improve-
ment of the reaction kinetics (hydrogen fuelling and refuelling
rates) and of the hydrogen transport properties can be achieved
by synthesizing MgH2 with a crystallite size in the nanome-
ter range by solid-state reaction through ball milling [7]. In the
investigation of the long and short range dynamics of hydrogen,
sorption kinetics, microstructure evolution and stability (grain
growth), role of added catalysts, the mechanical spectroscopy
may be fruitfully employed in synergy with other techniques
such as differential scanning calorimetry and X-ray diffraction
(XRD). The results shown in Fig. 3 refer to a samples of MgH2
in the form of a bar obtained by uniaxial pressing nanocrys-
talline powders prepared by reactive milling of Mg in hydrogen
atmosphere [8], and illustrate a case where both relaxational and
structural damping processes occur.

Fig. 3. Internal friction Q−1 and resonant frequency f of nanocrystalline MgH2
during successive thermal runs.
Fig. 4. (a) Internal friction Q−1 and dynamic Young’s modulus E for aluminium-
foam (solid circle) and a fully dense polycrystalline 4N-Al sample (grey circle);
in the inset are shown the Q−1 peaks after background subtraction. (b) Fitting of
the background damping at high temperatures for two foams (open triangle and
solid circle) measured at the frequencies indicated and the fully dense aluminium
sample (grey).
546 S. Amadori et al. / Materials Science and Engineering A 442 (2006) 543–546
on aluminium foams prepared by the method developed at
the Fraunhofer Institut in Bremen, starting from a mixture of
aluminium powders, TiH2 powders (blowing agent) and SiC par-
ticles (stabilizer) [11,12]. The samples have a relative density of
0.2. As shown in Fig. 4(a) the aluminium foam measured at very
low strain amplitude, <10−5 , shows a background damping of
1–2 × 10−3 up to 100–150 K, which is lower than that of dense
polycrystalline aluminium by a factor 2 in the present case. The
low-temperature background damping of foams increase up to
4–5 × 10−3 , becoming comparable to those of fully dense poly-
crystalline 4N-aluminium, when strains up to 10−4 are reached.
The high-temperature background damping, Fig. 4(b), exhibits
well a simple exponential trend, Q−1 = A exp(−B/kT), in the
temperature (T) interval 450–700 K. The fit to the experimental
data gives an apparent average activation energy, B ∼ 0.20 eV,
whereas in the bamboo boundary-polycrystalline 4N-aluminium
a slightly higher value, B ∼ 0.30 eV, is obtained (see Fig. 4(b)).
6. Conclusions
The mechanical analyzer presented here exhibits specific
advantages for the measurement of dynamic moduli of elasticity
and damping factor of materials. The high sensitivity of the reso-
nant vibrating-reed apparatus is coupled to the complete automa-
tion, high vacuum conditions, extended temperature range, rate
of data acquisition, real-time analysis and data display. These
requirements make it the better choice for mechanical charac-
terization of several technological materials, as put forward by
the reported case studies.
Acknowledgements
This research was partly supported by ‘Istituto Nazionale per
la Fisica della Materia’ (INFM) and CANTIL SrL.
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