Impulse excitation apparatus to measure resonant frequencies, elastic

moduli, and internal friction at room and high temperature

G. Roebben, B. Bollen, A. Brebels, J. Van Humbeeck, and O. Van der Biest

Citation: Rev. Sci. Instrum. 68, 4511 (1997); doi: 10.1063/1.1148422

View online: http://dx.doi.org/10.1063/1.1148422
View Table of Contents: http://rsi.aip.org/resource/1/RSINAK/v68/i12
Published by the American Institute of Physics.

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 Impulse excitation apparatus to measure resonant frequencies, elastic
moduli, and internal friction at room and high temperature
G. Roebbena)
Department of Metallurgy and Materials Engineering, Katholieke Universiteit Leuven, de Croylaan 2,
B-3001 Heverlee, Belgium
B. Bollen
Integrated Material Control Engineering, Wetenschapspark 1, B-3590 Diepenbeek, Belgium
A. Brebels
C.I.T. vzw, Kleinhoefstraat 4, B-2440 Geel, Belgium
J. Van Humbeeck and O. Van der Biest
Department of Metallurgy and Materials Engineering, Katholieke Universiteit Leuven, de Croylaan 2,
B-3001 Heverlee, Belgium
~Received 28 April 1997; accepted for publication 3 September 1997!
This paper presents a new apparatus to measure elastic properties and internal friction of materials.
The apparatus excites the test specimen by a light mechanical impact ~impulse excitation! and
performs a software-based analysis of the resulting vibration. The resonant frequencies f r of the test
object are determined and, in the case of isotropic and regular shaped specimens, the elastic moduli
are calculated. The internal friction value (Q 21 ) is determined for each f r as Q 21 5k/( p f r ) with
k the exponential decay parameter of the vibration component of frequency f r . A furnace was
designed and equipped with automated impulse excitation and vibration detection devices, thus
allowing computer-controlled measurements at temperatures up to 1750 °C. The precision of the
measured f r depends on the size and stiffness of the specimen, and varies from the order of 1023
~that is 61 Hz at 1 kHz! in soft, high damping materials or light specimens, to values as precise as
1025 ~that is 60.1 Hz at 10 kHz! in larger or stiffer specimens. The highly reproducible Q 21
measurements are accurate whenever the relation Q 21 5k/( p f r ) holds. The precision of the Q 21
measurement depends on the suspension or support of the specimen, and on the specimen size. Since
external energy losses are relatively smaller for larger specimens, the lower limit of measurable Q 21
extends from 1023 for small specimens ~for example ,1 g! down to 1025 with increasing specimen
size. High temperature tests have shown that Q 21 can be monitored up to values of about 0.1.
© 1997 American Institute of Physics. @S0034-6748~97!00412-7#

I. INTRODUCTION class of materials to the other.3 In general, the hysteretic

A. Resonant frequencies, elastic moduli, and internal
friction
Solid objects have a characteristic set of mechanical
resonant frequencies ( f r ) which are related to the object’s
mass, dimensions and elastic properties. In the case of mono-
lithic, isotropic specimens of simple geometry, this relation
is straightforward. Therefore, measurement of f r allows in-
vestigation of the elastic properties E, G and n and their
changes as a function of microstructural or extensive para-
meters such as temperature. For objects with complex
shapes, or made of anisotropic materials, or consisting of
multiple components, the relation is not as simple. Neverthe-
less, f r can be measured to characterize the object numeri-
cally. Already in 1937 Förster recognized such resonance
frequency measurement as a powerful tool in quality
control.1
The vibration can also be analyzed from the internal fric-
tion (Q 21 ) point of view,2 i.e., the dissipation of vibration
energy in the specimen, or damping, or mechanical loss.
Q 21 can be deduced from the amplitude decay of a free
vibration. The microstructural origin of Q 21 varies from one
a!
Electronic mail: gert.roebben@mtm.kuleuven.ac.be
rearrangement of microstructural features upon application
of a dynamic load causes internal friction. Examples are the
motion of interstitial carbon atoms in steel, and oxygen va-
cancies in zirconia crystals, the realignment of glass mol-
ecules or polymer chains, and dislocation interface move-
ment in crystalline solids. Also larger structural defects like
cracks or delaminations can induce energy loss through fric-
tion. An important feature of Q 21 in a homogeneous speci-
men is the fact that it is essentially independent of the geo-
metry of the solid. This means that Q 21 can be used in
process control as information additional to f r , which does
depend on the geometry of the object.
B. The impulse excitation technique
Several types of apparatus exist which measure the f r
and/or Q 21 of solid objects.4 Some of these systems rely on
an impulse excitation to induce the vibration: a light impact
is given to the specimen that, after a short transient period,
will vibrate at one or more of its resonant frequencies.
This impulse excitation technique ~IET! is essentially
non-destructive,5 can be applied at high temperatures and in
aggressive atmospheres, and requires no special shape for the
tested specimen. IET has found world-wide acceptance both
in industry and research.5–10 This paper presents a new IET
apparatus, available from IMCE ~see author’s affiliations!.

Rev. Sci. Instrum. 68 „12…, December 1997 0034-6748/97/68„12…/4511/5/$10.00 © 1997 American Institute of Physics 4511

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 FIG. 1. Example: ~a! Flexural and ~b! torsional vibration mode of rectangu-
lar bars.
II. DESCRIPTION OF THE NEW IMPULSE-EXCITATION
APPARATUS
A. Impulse excitation and vibration detection
The vibration modes of a specimen depend on its shape,
the place of impact and the type of support. Since these
modes are well defined for simple shapes ~bars, rods, disks,
...!, the supports can be placed in the nodes of the desired
vibration mode. Figure 1 ~a for flexural and b for torsional
vibration! shows how to support the specimen in these
nodes, thus minimizing the frictional losses at the supports.11
Measurements are mainly performed in the flexural mode,
using two setups. The first one has supports made of a
polymer-foam cylinder (B 5 mm!, glued to steel blocks that
are clamped to a heavy mounting table to reduce the influ-
ence of external vibrations @Fig. 2~a!#. A second setup is
mounted on a pallet and can be bottom-loaded into the fur-
nace. In this set-up the specimen lies on platinum-rhodium
~PtRh! wires that are fixed to parallel alumina ~Al2 O3 ) rods
@Fig. 2~b!#. During long term tests, Al2 O3 rods are hanging
from additional PtRh wires that lie on top of the specimen to
prevent the shift of the specimen upon repeated mechanical
impact.
The place of impact is near an antinode of the vibration.
The impact can be provided manually, with a simple tool
consisting of a steel ball glued to the end of a flexible poly-
mer rod. The excitation can also be performed pneumati-
cally, by firing a small light ceramic cylinder at the speci-
men. After impact the cylinder drops back into the
pneumatic channel and is ready for the next measurement.
Tests have been successfully performed with the pneumatic
system on a specimen as small as 25 3 6 3 0.85 mm3 ,
weighing less than 1 g.
The specimen vibration is recorded by a piezo crystal or
4512 Rev. Sci. Instrum., Vol. 68, No. 12, December 1997
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FIG. 2. ~a! Test specimen with impulse excitation and vibration detection
tools on the polymer-foam support, ~b! the PtRh-wire suspension unit as
used for high temperature tests.
by a microphone. A piezo crystal requires contact with the
specimen. Especially in the case of light specimens, the place
of contact has to be as close as possible to the vibration node
in order not to affect f r . In any case, the contacting piezo
crystal does not allow accurate measurement of Q 21 in light
specimens. Instead one can use a microphone, a non-
contacting transducer. For high temperature tests one end of
a ceramic tube is placed close to the specimen surface. The
tube guides the acoustic wave from the specimen out of the
furnace to a microphone.12 Laser vibrometry is currently be-
ing investigated for vibration detection in noisy or vacuum
surroundings, or of distant specimens.
B. Furnace
A furnace was built to perform impulse excitation tests
up to 1750 °C air at atmospheric pressure ~Super Kanthal
1800 heating elements, inner volume 215 3 120 3 165
mm3 ). A Pt30%Rh / Pt6%Rh thermocouple is used to mea-
sure the temperature of the test specimen. An Al2 O3 shell
around the test specimen provides an indirect and homoge-
neous heating of the specimen.
The waveguide tube enters the furnace from its top. Also
through this feedthrough the beam of a laser vibrometer can
reach the specimen surface. The ceramic tube through which
the impacting projectile is fired at the specimen enters the
furnace via a hole through the bottom-loaded pallet. A sec-
ond hole in the pallet can be used to lead an inert gas flow
~N2 , Ar, ...! into the Al2 O3 shell to prevent excessive oxida-
tion at the higher temperatures. A furnace with controlled
inert or vacuum atmosphere is in preparation.
Elastic properties
 TABLE I. Q 21 and f r of the flexural vibration of an annealed rectangular TABLE II. Q 21 and f r of flexural and torsional vibration of an Al2 O3
99.99% Cu bar. specimen in two support modes.

f r ~Hz! k~1/s! E~GPa! Q 21 Vibration Support fr k E G

mode mode ~Hz! ~1/s! ~GPa! ~GPa! Q 21
3959 12.1 119 0.000 97
3960 11.3 119 0.000 91 Flexural Flexural 8249 6.5 347.5 – 0.000 25
3961 12.4 119 0.001 00 Flexural Torsional 8249 18.2 347.5 – 0.000 70
3959 12.3 119 0.000 99 Torsional Flexural 18352 15.3 – 144.6 0.000 27
Torsional Torsional 18352 6.7 – 144.6 0.000 12

C. Signal analysis
The so-called resonant frequency and damping analyzer
amplifies and adapts the transducer signal, which then is
stored by a PC. A program written in LabVIEW™ ~registered
trademark of the National Instruments Corporation! deter-
mines the f r by Fourier analysis. The program assigns a
vibration of the form x(t)5Ae 2kt sin(2p f rt1f) to each f r
that is judged relevant by the operator. An algorithm simu-
lates the measured signal as a sum of these transient sinu-
soidal waves, optimizing iteratively the parameters A, k, f r
and f . Having reached a pre-selected convergence criterion,
the program gives the final f r , and for each of them a value
k. If the specimen shape, dimensions and mass are known,
the elastic moduli are calculated from the f r using the rela-
tions prescribed by ASTM C 1259-94.5 For each k the cor-
responding Q 21 is calculated as Q 21 5k/( p f r ).4
III. TEST MEASUREMENTS
A. Accuracy of the measurement: computer
simulation tests
Computer-generated electric signals composed of se-
veral exponentially decaying sinusoidal components to simu-
late specimen vibration, were used to test the accuracy of the
extraction algorithm. The frequency determination is perfect
up to a level of 0.001 Hz, and k is measurable in a Q 21
range of 0.000 01 to 0.1. This means that the apparatus de-
livers highly accurate Q 21 values whenever the relation
Q 21 5k/( p f r ) holds, i.e., if Q 21 ,0.1.4
B. Impulse excitation tests at room temperature
1. Reproducibility of the measurement
Manual impulse excitation tests are performed on an an-
nealed copper ~Cu! bar ~60.1 3 4.4 3 3.8 mm3 , 8.6885 g! on
the polymer-foam support. From the results ~Table I! one
concludes that f r can be determined with a repeatability in
the order of 1 Hz. This variation is too small to affect the
accuracy of the calculated elastic modulus @Eq. ~1!#, which is
dominated by the accuracy of the bar’s width b and length L,
but especially by its thickness t.5
was expected for pure Cu ~bending test, frequency 100
Hz!,14 hence three times as high. It must be emphasized that
Q 21 is not only severely dependent on the material’s micro-
structure, but also varies with the vibration frequency and
amplitude.
2. Limits to the measurement’s precision: external
friction
A basic assumption is made: the measured Q 21 cannot
underestimate the real one, since every measurement is af-
fected by extra energy losses which add to the real Q 1 .4 To
determine the contribution of the external energy losses tests
were performed on dense monolithic ceramics, materials
which are known to exhibit very low Q 21 at room tempera-
ture.
a. Influence of support position
While the exact location of the support has only a small
influence on f r , it has a large effect11 on the measured Q 21 .
If the supports are not located right at the nodes, Q 21 in-
creases substantially. Before each test the specimen supports
therefore have to be moved gradually towards the nodes by
minimizing Q 21 . A higher Q 21 is expected for the vibration
components that do not correspond to the chosen specimen
support. This is confirmed by the data in Table II, obtained
on an Al2 O3 specimen ~150.4 3 25.5 3 19.8 mm3 , 288 g!,
resting on polymer supports of the types shown in Figs. 1~a!
and 1~b!. In contrast, f r and hence the elastic moduli values
hardly seem to be affected.
b. Influence of support system
Two quartz specimens ~nominally 60 3 10 3 3 mm3,
dimensional accuracy better than 1%! were tested, both on
the Pt-wire suspension, and on the polymer-foam supports.
Since quartz exhibits a Q 21 less than 1025 ,14 the measured
Q 21 can be fully attributed to ‘‘external’’ friction. The re-
sults ~Table III! show that the thin wire support causes far
~53!
TABLE III. Average Q 21 and f r for several tests on two quartz specimens
in flexural vibration on two different supports ~standard deviations between

E5 0.9465 S m~ f r!2
b DS D
L3
T .
t3 1
~1!
brackets!.

Wire suspension Polymer-foam support

In Eq. ~1! m is the specimen weight. The correction factor T 1 Specimen f r ~Hz! k~1/s! Q 21 (31023 ) f r (Hz) k~1/s! Q 21 (31023 )
depends on the ratio L/t and the Poisson’s ratio ~0.35 for
Cu!, and was calculated to be 1.029. The calculated E ~119 No. 2 4875.3 0.96 0.063 4874.0 4.90 0.320
~0.1! ~0.03! ~0.002! ~0.1! ~0.01! ~0.001!
GPa! corresponds well with the expected value.13 No. 3 4901.5 0.73 0.047 4899.9 4.50 0.292
The standard deviation on the Q 21 measurements is ~0.5! ~0.01! ~0.0005! ~0.1! ~0.02! ~0.001!
about 5% of the mean value 0.000 97. A loss factor of 0.003

Rev. Sci. Instrum., Vol. 68, No. 12, December 1997 Elastic properties 4513

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 TABLE IV. Average Q 21 and f r ~and E) of a series of tests on an as TABLE V. Average Q 21 and f r of the flexural vibration of large Si3 N4
sintered and an annealed Si3 N4 specimen in flexural vibration ~oop 5 out of specimens ~standard deviation between brackets!.
plane, ip 5 in plane, standard deviation between brackets!.
fr k Q21
f r,oop E oop k oop Q 21
oop f r,ip E ip Si3N4 „Hz… „1/s… „31023)
Si3N4 ~Hz! ~GPa! ~1/s! (31023 ) ~Hz! ~GPa!
As sintered 2154 0.7 0.11
As sintered 15 025.3 299.6 8.1 0.17 19 768.3 299.6 ~1! ~0.1! ~0.005!
~0.1! ~0.1! ~0.005! ~0.1! annealed 2157 0.7 0.10
Annealed 15 093.9 302.3 7.3 0.15 19 870.2 302.9 ~2! ~0.1! ~0.005!
~0.1! ~0.1! ~0.005! ~0.2!

specimen is removed from its support. Comparing the Q 21

less external friction than the polymer-foam support unit data in Table IV and Table V shows that in larger specimens
does. A second but smaller difference is observed between the ratio of external friction to ‘‘internal’’ friction becomes
the Q 21 of the two specimens, which is tentatively explained smaller: the value of parasitic damping decreases with in-
by small differences in the roughness of the machined side creasing specimen size.
surfaces. The level up to which the Q 21 measurements are
reproducible ~of the order of 1026 ) is smaller than the exter- 3. High-damping materials
nal friction contribution ~of the order of 1024 ). Hence, the
Some metals have a high Q 21 at room temperature, as
accuracy of Q 21 is entirely determined by the latter. This has
can be seen from the results of the tests on zinc ~Zn! and lead
to be accounted for when performing high precision Q 21
~Pb! beams ~Table VI!. The Q 21 values are large enough to
measurements, but it does not harm comparative measure-
neglect the contribution of the energy losses in the support.
ments of Q 21 . Parallel with the increased Q 21 measured on
Q 21 for the Pb specimen falls within the expected range.14
the polymer-foam support, a decrease in the f r is observed.
The literature values14 for Zn are smaller than the ones in
This can be the effect of the extra external friction. The
Table VI, probably due to differences in the material micro-
influence, however, is smaller ~of the order of 1024 ) than the
structure and in vibration amplitude and frequency.
accuracy on the dimensions of standard machined speci-
mens, and would not affect the calculation of the elastic
C. Elevated temperature scans
moduli.
1. Oxide ceramics
c. Influence of specimen size A polycrystalline Al2 O3 specimen ~size 83 3 12.5 3 3
The effect of specimen size was investigated by per- mm3 , weight 9.3 g! was tested. Figure 3 shows the evolution
forming tests on two types of silicon nitride ~Si3 N4 ) speci- of f r ~and E) and Q 21 from room temperature to 1500 °C. It
mens. First accurately machined bars ~nominally 44 3 4 3 3 is known from literature that no sudden changes in both E or
mm3 , dimensional accuracy better than 0.1%! of an as sin-
TABLE VI. Results of tests on Zn and Pb specimens at room temperature.
tered and a heat treated Si3 N4 were tested on the wire sus-
pension unit. Table IV shows that the annealing heat treat- weight dimensions f E k
ment ~5 h at 1420 °C! induces a stiffening of the ceramic specimen ~g! ~mm! ~Hz! ~GPa! ~1/s! Q 21
~13 GPa!. This agrees with the results of uniaxial tests and
Pb 37.7 56.7 3 12.0 3 5.0 2239.8 22 115 0.0164
other resonant frequency tests, and is the result of devitrifi- Zn 29.1 60.7 3 12.4 3 5.6 4970.2 74 473 0.0303
cation of the 10 vol % intergranular region.15 Notice the
agreement of the out-of-plane ~oop! and the in-plane ~ip!
measurements ~oop: impulse on the 3 3 44 mm2 side of the
specimen, ip: impulse on the 4 3 44 mm2 side of the speci-
men!, even though during both measurements the specimen
was suspended in the oop position. Q 21 is only marginally
different between as sintered and annealed Si3 N4 . We found
in the literature14 a loss factor of 0.000 025 for Si3 N4 , which
is one order of magnitude smaller than the values in Table
IV. This confirms that the latter are due to external friction,
presumably in the specimen support.
Secondly, tests were performed on larger specimens with
a flat waisted shape ~outer dimensions 160 3 20 3 6 mm3 ).
Small dimensional irregularities induce a slightly different f r
for each specimen and obscure the difference in f r ~and E)
between the as sintered and the annealed specimens ~Table
V!. Q 21 is determined with a sensitivity of 1025 over a
series of specimens, and does not differ significantly between
the as sintered specimens and the heat treated specimens. No FIG. 3. The resonant frequency f r and internal friction value Q 21 in
differences can be discerned when between measurements a Al2 O3 as a function of temperature.

4514 Rev. Sci. Instrum., Vol. 68, No. 12, December 1997 Elastic properties

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 FIG. 5. E and Q 21 in Si3 N4 as a function of temperature.

duction of the Q 21 peak near T g . This indicates crystalliza-

21
FIG. 4. The resonant frequency f r and internal friction value Q in ZrO2 tion of the intergranular phase. The same Si3 N4 was tested in
as a function of temperature. a torsion pendulum19 and uniaxially,20 revealing good agree-
ment between the torsion pendulum and the IET results.
Q 21 of a pure Al2 O3 occur at temperatures below 1000 °C.
Above this temperature the grain boundary defects become
mobile, and minor secondary phases soften.16 This leads to ACKNOWLEDGMENTS
the increase of Q 21 and a corresponding decrease in f r , The research was performed with the support of the
which agrees with the results presented in Fig. 3. Above a Flemish Institute for the Promotion of the Scientific Technol-
certain Q 21 ~6%!, the vibration amplitude decreases too fast ogy Research in Industry ~IWT!. One of the authors ~G. R.!
to allow accurate analysis. This is close to the 10% level thanks the IWT for a grant. The authors acknowledge the
above which the anelastic assumptions required to calculate Institute for Advanced Materials, Petten, the Netherlands, for
Q 21 from k are not valid anymore. having provided the Si3 N4 specimens.
Also a polycrystalline zirconia ~ZrO2 ) was tested in air.
The crystal lattice of ZrO2 contains substitutional Y31 or
Mg21 cations, and corresponding charge compensating oxy- 1
F. Förster, Z. Metallkd. 29, 109 ~1937!.
gen vacancies. Pairs of oxygen vacancies and substitutional
2
ASTM E 756-83, Am. Soc. Testing and Materials ~1984!.
3
R. De Batist, in Materials Science and Technology: A Comprehensive
ions constitute elastic dipoles, which reorient under applied Treatment ~VCH, Weinheim, Germany, 1994!, Vol. 2B, Chap. 12.
stress.17 The motion of these pairs and larger agglomerates is 4
A. S. Nowick and B. S. Berry, in Anelastic Relaxation in Crystalline
thermally activated and well defined, which explains the sud- Solids ~Academic, New York, 1972!.
5
ASTM C 1259-94, Am. Soc. Testing and Materials ~1994!.
den decreases in f r and sharp Q 21 peaks in the correspond- 6
J. W. Lemmens, ASTM STP 1045, Am. Soc. Testing and Materials
ing temperature scans ~Fig. 4!. ~1990!, p. 90.
7
L. S. Cook, A. Wolfenden, and G. M. Ludtka, ASTM 1045, Am. Soc.
2. Non-oxide ceramics Testing and Materials ~1990!, p. 75.
8
L. Chandra and T. W. Clyne, J. Mater. Sci. Lett. 12, 191 ~1993!.
9
Si3 N4 is a structural ceramic, like Al2 O3 , but cannot be M. Sakata, K. Kimura, and A. Mizunuma, J. Am. Ceram. Soc. 78, 3040
pressureless sintered to full density without a considerable ~1995!.
10
Z. Zhang, D. Jin, L. Li, Z. Tu, L. Zhao, P. Zhang, and J. Zhao, J. Am.
amount of sintering additives, unlike Al2 O3 . Therefore pres- Ceram. Soc. 78, 2548 ~1995!.
sureless sintered Si3 N4 contains a secondary, intergranular 11
J. B. Wachtman, Jr., and W. E. Tefft, Rev. Sci. Instrum. 29, 517 ~1958!.
phase. This phase is ~partially! amorphous, and softens 12
K. Heritage, C. Frisby, and A. Wolfenden, Rev. Sci. Instrum. 59, 973
above its glass transition temperature T g ~typically near ~1988!.
13
Metals Handbook, ~ASM International, 1990!, Vol. 2.
1000 °C!. This triggers viscous deformation of the bulk ce- 14
J. Zhang, R. J. Perez, and E. J. Lavernia, J. Mater. Sci. 28, 2395 ~1993!.
ramic, and consequently increases Q 21 . At temperatures too 15
G. Roebben, L. Donzel, M. Steen, R.Schaller, and O. Van der Biest, Euro
far above T g the secondary phase does not resist the defor- Ceramics V, Key Engineering Materials ~Trans Tech, Zürich, 1997!, Vols.
132–136, p. 655.
mation anymore. Less energy is dissipated since deformation 16
A. Lakki, dissertation, École Polytechnique Féderale de Lausanne, 1994.
is blocked by the rigid Si3 N4 grains. When the temperature is 17
M. Weller, H. Schubert, and P. Kountouros, in Science and Technology of
increased even more, other diffusion-types of deformations Zirconia V ~Technomic, Lancaster, and Basel, 1993!, p. 546.
start playing a role, and Q 21 increases again.18 This behavior R. L. Tsai, and R. Raj, J. Am. Ceram. Soc. 63, 513 ~1980!.
18
19
G. Roebben, L. Donzel, S. Sakaguchi, M. Steen, R. Schaller, and O. Van
agrees well with the data presented in Fig. 5. der Biest, Scri. Metall. Mater. 36, 165 ~1997!.
One notices that the exposure to high temperature during 20
G. Roebben, M. Steen, and O. Van der Biest, Scri. Metall. Mater. 33, 1417
consecutive impulse excitation tests induces a substantial re- ~1995!.

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