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Automated Resonant Vibrating-Reed Analyzer Apparatus For A Non-Destructive Characterization of Materials For Industrial Applications
Automated Resonant Vibrating-Reed Analyzer Apparatus For A Non-Destructive Characterization of Materials For Industrial Applications
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
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
2. Experimental
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. 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
Fig. 3. Internal friction Q−1 and resonant frequency f of nanocrystalline MgH2 solid circle) measured at the frequencies indicated and the fully dense aluminium
during successive thermal runs. sample (grey).
546 S. Amadori et al. / Materials Science and Engineering A 442 (2006) 543–546