Inverse Ultrasonic Determination of Imperfect Interfaces and Bulk Properties of A Layer Between Two Solids

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Inverse ultrasonic determination of imperfect interfaces

and bulk properties of a layer between two solids


A. Baltazar, L. Wang, B. Xie, and S. I. Rokhlina)
Nondestructive Evaluation Program, Edison Joining Technology Center, The Ohio State University,
1248 Arthur E. Adams Drive, Columbus, Ohio 43221

共Received 5 March 2003; revised 8 June 2003; accepted 23 June 2003兲


A method for determination of the complete set of physical, geometrical, and interfacial properties
of an isotropic layer embedded between two known solids is discussed. These properties are: Lamé
elastic moduli, density and thickness of the layer, and complex normal and transverse interfacial
stiffnesses between the layer and the substrates. The properties are combined in the form of eight
nondimensional parameters, which are determined from experimental reflection spectra at two
incident angles: normal and oblique. The conditions for simultaneous determination of bulk layer
properties and the interface normal and transverse springs with losses and the stability of the
inversion method against data scatter are addressed. The inversion model is validated by experiment
on normal and angular ultrasonic reflectivity from a layer between two semispaces in dry
mechanical contact and from an environmentally degraded adhesive joint. The layer properties were
measured independently, showing good agreement with the reconstructed results. © 2003
Acoustical Society of America. 关DOI: 10.1121/1.1600723兴
PACS numbers: 43.35.Cg, 43.20.El, 43.35.Zc 关YHB兴

I. INTRODUCTION trasonic signatures perturbed by the interface. Both bulk and


guided waves were used for this purpose. The reflection re-
Modern materials are often engineered as layered struc- sponse from an elastically perfect interface is frequency in-
tures such as thin films in electronic parts, coatings for ser- dependent while from an interface with spring boundary con-
vice life extension, and advanced composite laminates. Also, ditions it depends on frequency. By measuring this frequency
different parts are often joined using thin layers, for example, response one can determine the interfacial spring stiffness.
adhesive bonding, brazing, and diffusion bonding. Properties For example, in more recent studies Rokhlin et al.18 used the
of thin layers are often tailored to satisfy design requirements reflectivity method to characterize an imperfect interface be-
and thus should be measured as part of quality process con- tween a plasma spray coating and a substrate, and Guo
trol. The bond integrity and strength 共adhesion兲 between the et al.19 applied high-frequency line-focus acoustic micros-
layer and the substrate is most difficult to control during copy to characterize an imperfect interface between a thin
manufacturing and is difficult to measure nondestructively. film and a substrate. In these papers models have been de-
However, it is well known that the strength and life expect- veloped and applied in the inversion procedure to determine
ancy of many engineering structures depends critically on interfacial spring constants from the measured acoustic sig-
the bond integrity between structural components. Imperfec- natures.
tions along the bondline such as cracks, porosity, inclusions, Most previous work has focused on single imperfect in-
etc. can significantly degrade the performance of the joint. terface characterization. However, characterization of imper-
Very often the imperfections are confined to a very thin layer fect interfaces between a layer and two substrates is also
in the form of an interphase separating the joining materials important for many material joining and coatings applica-
which is difficult to characterize. Ultrasonic methods have tions, for example for adhesive bonds which deteriorate in a
been very promising for nondestructive evaluation of such humid environment predominantly along the adhesive/
interphases. adherend interface20 where a model with water-filled micro-
When the interphasial layer between the solids is thin disbonds was developed to describe damage by distributed
and the imperfections are flat, the interphasial layer can be transverse springs and to characterize the degradation. The
modeled as an infinitely thin interface connecting the solids distinctive feature of this type of material system is that the
by distributed springs to account for interfacial stiffness re- layer is thin, and the ultrasonic signals reflected 共normally or
duction due to imperfections; and analytically, such an inter- obliquely兲 from the front and back sides of the layer are not
face can be modeled using spring boundary conditions1 separated in the time domain and interfere. Thus, ultrasonic
where spring values have been related by a model to the spectroscopy may be applied to characterize two imperfect
microcrack distribution.1,2 Significant effort has been put into interfaces separated by a layer of thickness h. This problem
experimental and theoretical studies of ultrasonic wave inter- was addressed recently by Lavrentyev and Rokhlin,21 who
action with imperfect interfaces.1–24 The goal of these stud- used ultrasonic spectroscopy to evaluate the interfacial con-
ies was to characterize interface imperfections measuring ul- ditions from the spectra of longitudinal and shear waves re-
flected normally by the neighboring interfaces. They showed
a兲
Electronic mail: rokhlin.2@osu.edu that the frequencies at which the reflected spectrum minima

1424 J. Acoust. Soc. Am. 114 (3), September 2003 0001-4966/2003/114(3)/1424/11/$19.00 © 2003 Acoustical Society of America

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occur are sensitive to interfacial conditions, and, therefore,
may be used for their monitoring.
More recently, Baltazar et al.22,23 demonstrated experi-
mentally that the values of the interfacial normal and trans-
verse stiffness constants obtained from data acquired at nor-
mal incidence may be used to predict the dynamic response
of the interface even when the interrogating wave impinges
on the interface at oblique incidence, i.e., these two interfa-
cial stiffnesses describe the imperfect interface uniquely.
They also provided a theoretical description of the microme-
chanics of rough, contacting surfaces under static normal and
shear loads. In particular, they predicted the values for the
ratio between the normal and transverse interfacial stiffness
constants.
In our and other previous studies it was assumed that the
properties of the bondline layer are known and only imper-
fect interface properties need to be determined from the ex-
periment. However, in many cases the properties of the
bonding layer are also unknown. If the ultrasonic reflectivity
signature from such a layer has an anomaly it is important to
FIG. 1. 共a兲 Layer embedded between two solids with an imperfect interface
know if it is due to the interface 共adhesion兲 imperfections or consisting of two rough surfaces. Using spring approximation complex nor-
due to the layer properties anomaly. Thus, an inverse- mal K N (N/m3 ) and transverse K T springs replace imperfect interface. 共b兲
independent determination of these properties from the ex- Model with effective layer perfectly bonded to substrates. The layer has
same thickness but effective elastic moduli which are selected to match as
perimental ultrasonic signature is important. In this paper we closely as possible the reflected ultrasonic signatures.
address this problem both theoretically and experimentally.
The development is an extension of the inversion method
proposed by Lavrentyev and Rokhlin24 and extended by Equation 共1兲 represents continuity of stress ␴ ik and disconti-
Wang et al.,25 who performed reconstruction of all geometri- nuity of displacement u i at the interfaces; h is the layer
cal and acoustic properties of a layer perfectly embedded thickness. The properties of the interfacial contacts are de-
between substrates. scribed by normal K N (N/m3 ) and transverse K T complex
interfacial spring constants. At perfect 共welded兲 contacts be-
tween solids the spring constants approach infinity.
We consider the layer properties and the interfacial
II. INVERSION MODEL FOR THE RECONSTRUCTION
OF INTERFACIAL AND BULK LAYER PROPERTIES springs, in the boundary conditions 共1兲, to be unknown. We
assume that the substrate properties are known a priori and
A. Definition of independent parameters for the interfacial springs are the same on both interfaces be-
embedded layer with imperfect boundary conditions tween the layer and the substrates. We use six parameters24,25
Let us consider a solid layer imperfectly embedded be- to describe all unknown variables: bulk layer properties and
tween two solids as shown in Fig. 1共a兲. To characterize the two interfacial spring constants. Those parameters will be
interfaces and layer properties the normal and oblique ultra- reconstructed from measured normal and angular reflection
sonic reflection signatures are taken from the layer. Recon- ultrasonic spectra. The model includes in general ten param-
struction of the interfaces and the layer parameters is model eters: Lame’s constants ␭ and ␮, thickness h, density ␳, lon-
based. In the model the imperfect interface conditions be- gitudinal ␣ l and shear ␣ t attenuations, and the interfacial
tween the layer and the substrates are represented by distrib- normal and transverse complex spring constants
uted complex normal and shear springs as shown in Fig.
1共a兲. The spring model is quasistatic and valid for wave- ␭, ␮ , h, ␳ , ␣ l , ␣ t , K N ⫽K N⬘ ⫹iK N⬙ , K T ⫽K T⬘ ⫹iK T⬙ .
lengths larger than the dimensions of the interface disconti- 共2兲
nuities. Using this concept the boundary conditions between
the layer and the substrates are described as However, as discussed below, the attenuation in the
layer and the imaginary parts in the spring constants cannot
␴ zz 共 z⫽⫾h/2⫹0 ⫾ 兲 ⫽ ␴ zz 共 z⫽⫾h/2⫹0 ⫿ 兲 be separated, and therefore a total of eight parameters will be
considered to be unknown. Generalizing the procedure de-
⫽K N 关 u z 共 z⫽⫾h/2⫹0 ⫹ 兲 scribed in Refs. 24 and 25, from the parameters 共2兲 we de-
⫺u z 共 z⫽⫾h/2⫹0 ⫺ 兲兴 , fined two groups of nondimensional parameters. From the
共1兲 normal-reflection spectrum the following four nondimen-
␴ xz 共 z⫽⫾h/2⫹0 ⫾ 兲 ⫽ ␴ xz 共 z⫽⫾h/2⫹0 ⫿ 兲 sional parameters will be determined:

⫽K T 关 u x 共 z⫽⫾h/2⫹0 ⫹ 兲 Zl h␻0
Z n⫽ , H l⫽ , K̄ N ⫽K N / 共 ␻ 0 Z l 兲 , ␣ l , 共3兲
⫺u x 共 z⫽⫾h/2⫹0 ⫺ 兲兴 . Zs Vl

J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties 1425

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where Z l,s ⫽ ␳ o,s V l,sl is the acoustic impedance; the subscript
s denotes quantities belonging to the substrate; ␳ o is the
density of the adhesive and ␳ s is substrate density, V l is the
longitudinal velocity in the adhesive, and V sl that in the sub-
strate; K̄ N is the nondimensional complex normal interfacial
spring constant, and ␣ l is the longitudinal attenuation in the
thin layer. The angular frequency was chosen as ␻ 0
⫽1 ␮ s⫺1 for convenience. At oblique incidence an addi-
tional set of four nondimensional parameters is determined
Vl Vt
H t␪⫽ , H l ␪ ⫽ , K̄ T ⫽K T / 共 ␻ 0 Z t 兲 , ␣ t . 共4兲
V sl V st
Here, K̄ T is the complex nondimensional transverse interfa-
cial spring constant, V t is the shear velocity in the adhesive
and V st that in the substrate; Z t ⫽ ␳ V t , and ␣ t is shear attenu-
ation in the adhesive.
The energy loss at the interface is accounted for by
imaginary parts in the interfacial stiffness constants (K N,T
⬘ ⫹iK N,T
⫽K N,T ⬙ ) . Physically, the interfacial losses at the in-
terfaces depend on the ultrasonic scattering. Our analysis
shows that the imaginary parts in the complex springs pro-
duce the same effect on the reflection spectra as attenuation
in the thin embedded layer ␣ l , ␣ t and therefore they cannot
be separated by our method. Such separation may be pos-
sible if one considers a different frequency dependence of
these variables; however, this will require a much wider fre-
quency bandwidth of measurement than is used in our work.
Thus, depending on the physical conditions we assume that
only one of the pair of attenuations is unknown and used for
reconstruction: either the attenuation coefficients ␣ l , ␣ t in-
side the thin layer or the imaginary parts of the interfacial
spring constants; the other pair is considered to be known.
We further discuss this issue in Sec. IV.

B. Discussion of separation of interfacial from bulk FIG. 2. Effect of bulk and interfacial properties on the spectrum of the
layer properties reflected signal from the embedded epoxy layer between aluminum sub-
strates; 共a兲 Reflection coefficient 兩R兩 versus frequency. The solid line is for a
As demonstrated in Refs. 24 and 25, all properties of the thin epoxy layer embedded between two aluminum plates with imperfect
layer perfectly bonded to the substrates (K N⬘ ,K T⬘ ⫽⬁) can be interfaces (K N⬘ ⫽1⫻1014 N/m3 ). The dashed line is for the effective layer
reconstructed from the normal and oblique reflectivity spec- model with perfect interfaces and the reduced bulk longitudinal wave veloc-
tra. For this reason, to describe the imperfection of the inter- ity; it has been determined by matching of the reflection spectrum at first
minimum 共marked M ) of the layer with imperfect interfaces 共dashed line兲.
faces 共degradation兲 the effective layer model 关Fig. 1共b兲兴 was 共b兲 Shows by solid lines the shift of the reflection spectra minima versus
used.26 In this model the imperfectly embedded layer is re- interfacial spring stiffness (V L ⫽2.59 mm/ ␮ s, h⫽0.18 mm). The dashed
placed by an effective 共equivalent兲 which is perfectly bonded lines correspond to the effective-properties model as in 共a兲.
to the substrates. The layer has the same thickness, but with
effective elastic moduli which are selected to match as
closely as possible the reflected ultrasonic signatures; the ef- effective 共artificial兲 properties, and the second is one with
fective moduli 共ultrasonic velocities兲 will be smaller than the actual layer properties but imperfect bonding to the sub-
actual ones to account for the reduction of the interface stiff- strates.
ness. Adding interfacial properties as unknown variables in- To illustrate this issue, we will use, as an example, simu-
troduces additional unknown parameters to be determined. lated reflection spectra at normal incidence. Figure 2共a兲
Assuming that normal and angular reflection spectra are shows simulated reflection frequency spectra for layers with
measured, the first question to be addressed is: is the separa- two different longitudinal velocities assuming perfect and
tion of interfacial from bulk properties of the layer possible imperfect interfaces. The solid line is for a thin epoxy layer
in principle? In other words, is the problem unique or can the (h⫽0.18 mm, V L ⫽2.59 mm/ ␮ s) embedded between two
identical ultrasonic reflectivity signature be obtained from aluminum plates with imperfect interfaces (K N⬘ ⫽1
two different models: the first is the effective layer model ⫻1014 N/m3 ). The dashed line is calculated assuming per-
with a perfectly bonded layer between the substrates and fect interfaces and the reduced bulk longitudinal wave speed

1426 J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties

Redistribution subject to ASA license or copyright; see http://acousticalsociety.org/content/terms. Download to IP: 130.102.42.98 On: Sat, 22 Nov 2014 05:04:29
to V L ⫽1.53 mm/ ␮ s; it has been determined by inverse least-
squared optimization of the matching of the reflection spec-
trum at first minimum 共marked M ) of the layer with imper-
fect interfaces 共dashed line兲. We call the model, with such
matched properties of a perfectly bonded layer, the effective
layer model. As can be seen, only the first minimum position
is overlapped for these two cases; other minima cannot be
matched. The frequencies of the higher resonance minima
become significantly different for the two types of interfacial
conditions. Figure 2共b兲 shows by solid lines the shift of the
reflection spectra minima versus interfacial spring stiffness
(V L ⫽2.59 mm/ ␮ s, h⫽0.18 mm). The dashed lines corre-
spond to the effective-properties model. As in Fig. 2共a兲, to
obtain the effective layer velocity the least-squares spectra
inversion procedure was used to match the first resonance
minimum by the two models at each corresponding value of
the interfacial springs 关marked M in Fig. 2共b兲兴. Thus, for
both models the curves for the lowest resonance coincide.
The positions of the second and third minima are the same
for large values of interfacial stiffness 共i.e., K N⬘
⬎1015 N/m3 ); however, they become different as the inter-
facial stiffness is reduced.
This indicates that in the frequency band covering sev-
eral layer resonances the reflected spectra change differently
with change of bulk layer properties or change of the inter-
FIG. 3. Reconstruction procedure.
facial properties, and the effective layer model will not
match the reflected spectra for imperfect interface conditions
in a wide frequency range. On the other hand, performing spectrum from the imperfectly embedded layer used in the
measurements in a broad frequency range would permit de- reconstruction is deconvolved with the spectra of the refer-
coupling the effect of the interfacial stiffness from the layer ence signal. By this deconvolution, frequency and beam ef-
bulk properties. However, if only one spectral minimum is fects of the transducers are removed from the experimental
measured the effective layer model and the complete model spectra. If the experimental conditions are the same for both
with the interfacial springs give identical inversion results the specimen and reference signal measurements, the beam
and the interfacial springs cannot be separated from the layer effect due to the finite size of the transducer aperture is re-
bulk properties. moved and the plane-wave approximation may be employed
The reflection spectra resonances are formed due to mul- in the properties reconstruction.25
tiple reflections of the ultrasonic signal in the layer, and The flow chart for the reconstruction procedure for the
therefore they are sensitive to the interfacial conditions on parameters 共3兲 and 共4兲 is shown in Fig. 3. First, the normal
both interfaces. We do not intend to separate the conditions and oblique spectra are measured experimentally. Then, the
on these interfaces and assume them to be identical 共such a parameters defined in Eq. 共3兲 are obtained from the normal
separation is unlikely to be possible by this method兲. In our spectrum using a least-square optimization algorithm. These
experiment the surface preparation of the sample to form the reconstructed parameters are then used in a similar optimi-
two interfaces between the layer and the substrates is identi- zation procedure to obtain the rest of the parameters in Eq.
cal; therefore, our assumption that the interfacial springs on 共4兲 from the oblique reflection spectrum. After all nondimen-
both interfaces are identical is reasonable. Our simulations sional parameters have been determined, the dimensional pa-
show that when the interfacial properties are not symmetrical rameters 共2兲 are obtained from 共4兲 and 共5兲.22 Considering the
the reflection spectra behaves somewhat like that for the unknown nondimensional parameters as a variable vector X
symmetrical interfaces with averaged compliances. in a four-dimensional space, their values are calculated by
least-squares minimization of the sum of squared deviations
between the experimental R e (X0 ) and simulated R t (X) spec-
C. Inversion algorithm
tra
As described above, the reflection spectra depend on the
f2
two sets of nondimensional parameters defined by Eqs. 共3兲
and 共4兲 which are reconstructed from the experimental nor- Error共 X兲 ⫽min 兺
f⫽f1
共 兩 R t 共 X兲 兩 ⫺ 兩 R e 共 X0 兲 兩 兲 2 . 共5兲
mal and oblique reflection spectra by minimizing the match-
ing error between the measured and simulated spectra. A X is an iterated set of four unknown nondimensional param-
multilayered wave propagation algorithm24,25 with spring eters 关Eq. 共3兲 or 共4兲兴, X0 is the corresponding actual set of
boundary conditions between layers is used to compute the material properties 共interfacial and bulk layer properties兲. f 1
reflection spectra in the model. The experimental reflection and f 2 are the bounds of the frequency band in which mini

J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties 1427

Redistribution subject to ASA license or copyright; see http://acousticalsociety.org/content/terms. Download to IP: 130.102.42.98 On: Sat, 22 Nov 2014 05:04:29
FIG. 4. Cross sections of the 4D error function: 共a兲
K n⬘ – H l cross section for normal incidence measure-
ments. 共b兲 K ⬘t – H t ␪ cross section for oblique incidence
measurements.

mization is performed. The frequency bounds are selected guesses in the range of 20% off the actual values. Figure
based on the transducer bandwidth and the resonance 5共a兲 shows the scatter effect on H l and Fig. 5共b兲 for H l ␪ .
frequencies of the adhesive layer. Equation 共5兲 is applied The standard deviation for H l is within 0.5% and for H l ␪
separately to normal and oblique cases as specified in is 1%.
Fig. 3.
The least-square algorithm may converge to one of the
minima of the error function 共5兲 in the four-dimensional pa-
rameter space. The initial guesses and accuracy of the mea-
surement will affect the convergence of the algorithm and
may make it reach a local minimum rather than the global
minimum corresponding to the actual parameters. To inves-
tigate the influence of the initial guesses we calculated the
error function surface. As an example, two cross sections of
the error function in the form of gray level images are plotted
in Fig. 4. Black corresponds to the smallest level. The non-
dimensional parameters (K n and H l ) in Fig. 4共a兲 and (K t and
H t ␪ ) in Fig. 4共b兲 are normalized and allowed to vary from
50% to 150% of the actual parameters K n0 , H l0 , K t0 , H t ␪ 0 .
Other parameters are kept at the actual value. As can be seen,
only one main minimum exists within this range of variation.
This indicates that the least square minimization process 共5兲
converges to the actual parameters if the initial guesses are
selected within the above variation range and there is no data
scatter. Contours of error magnitudes form ellipses, indicat-
ing that the rate of convergence depends on the direction of
search and the initial guesses. Similar results were obtained
for all other parameters.
The inverse problem discussed above depends on the
measurement accuracy of both the normal and angular reflec-
tion spectra. To assess the effect of data scatter we employed
the algorithm described by Wang et al.,25 who used a ‘‘noisy
spectrum’’ obtained by introducing random scatter into the
time-domain signal calculated by the beam model which
emulates experimental conditions in the angle beam
measurements.25 The simulated experimental signal has been
mixed with random ‘‘noise’’ data. The amplitude of random
data scatter is 2% of the signal peak amplitudes. Due to
data scatter the reconstructed set of layer properties is
not exactly equal to the original set. The difference serves as
a measure of the effects of the data scatter level and the
quality of initial guesses on the inversion algorithm. As
an example, in Figs. 5共a兲 and 共b兲, we plot the relative error
FIG. 5. Histograms for repeated 200 times reconstructions with synthetic
between the reconstructed parameter values and the exact ‘‘noisy’’ time domain signals 共2% scatter兲. Initial guesses are 20% off the
original values as histograms for 200 times repeated recon- actual values. 共a兲 Results for H l for normal incidence measurement; 共b兲
structions for the same data scatter 共2%兲 and different initial result for H l ␪ for oblique incidence measurement.

1428 J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties

Redistribution subject to ASA license or copyright; see http://acousticalsociety.org/content/terms. Download to IP: 130.102.42.98 On: Sat, 22 Nov 2014 05:04:29
nominal contact area and load level produced a range of
applied pressure between 0– 46 MPa. The contacting sur-
faces of the thin plates as well as aluminum substrates
共blocks A and B兲 were roughened with 600⫻-grit sandpaper.
Examining the surfaces after roughening showed a random
distribution of asperities with an rms roughness of about 0.3
microns.
Three longitudinal wave transducers were positioned in
the upper aluminum block: two for oblique incidence in
pitch–catch mode and one for normal incidence in echo–
pulse, as can be seen in Fig. 6. Transducers were all selected
as broadband with central frequency 20 MHz; this allowed
the presence of more than one resonance minimum in our
experiments. The external loading was controlled via a Ma-
terial Test System model 810, and the system operated in the
range of applied load 0–10 klb 共0– 44.5 kN兲.
A critical part of the experiment is careful alignment of
the contacting surfaces to obtain parallelism of the surfaces
FIG. 6. Experimental setup for the determination of normal and oblique in contact; otherwise, nonuniformity of the interfacial stiff-
reflection signals from a thin layer embedded between two aluminum blocks ness along the contact area might take place 共the misalign-
under controlled load.
ment effects have been discussed in detail in Ref. 27兲. To
facilitate alignment, the lower part of the system 共Fig. 6兲 has
III. EXPERIMENT a hemispherical support; this allows two rotational degrees
The key element of this study is to validate experimen- of freedom while providing normal force transfer.
tally the reconstruction algorithm and to demonstrate the Ultrasonic reflected signals were captured and digitized
separation of the bulk layer bulk properties from those of the for further analysis as a function of the load cycle. The re-
interface. To do this we need the ability to measure the prop- flected spectra from the interface at each loading level were
erties by independent techniques, which is a difficult task. deconvolved with the reflected spectrum from the free sur-
We partially solved this problem by specially designing the face.
experiments and using thin layers with independently mea-
sured properties and by obtaining controllable interfacial
conditions between the layer and the substrates. 2. Reflectivity spectra

A. Thin layer in dry contact between substrates The use of a thin aluminum layer between aluminum
substrates allows isolating the effect of interfacial stiffness
1. Experimental procedure on reflected ultrasonic signals by eliminating the impedance
In one series of experiments the measurements were per- mismatch between the layer and the substrates. When the
formed on a sample with a thin aluminum layer positioned in thin plate and substrates have the same properties, the posi-
dry contact between two aluminum substrates. The interfa- tion and amplitude of the reflection minima will depend only
cial contacts are controlled by applying predetermined pres- on the interface stiffness, which is allowed to change from
sure on the layered system. The bulk properties of the thin zero, at complete disbond, to infinity for perfect interface
layer are measured independently; they do not change under conditions; in this last case the reflection is zero. Lavrentyev
pressure, but the interfacial contacts vary significantly.21–23 and Rokhlin21 investigated the application of the spring
Our objective is to reconstruct these bulk and interfacial model to model the reflected signature from normal inci-
properties from ultrasonic measurements and to compare the dence of longitudinal waves, and established that the fre-
reconstructed bulk properties with the original ones. The re- quency minima shift can be used to estimate the normal in-
sult of this comparison serves as a measure of the quality of terfacial stiffness.
the reconstruction of the properties including those of the Experimental results for the aluminum/aluminum layer/
interfaces. aluminum system using longitudinal waves at normal and 38
The experimental setup is depicted in Fig. 6; this in- deg oblique incidence versus pressure on the sample are
cludes the mechanical system with load control, ultrasonic given in Fig. 7. Results are for nominal pressures ranging
pulser/receiver and transducers, and signal acquisition sys- from 10 to 24 MPa with increments of 2 MPa. The reflected
tem. The system is self-aligned, allowing homogeneous load- spectra from normal as well as oblique incidence shift to
ing distribution at the contacting area. It is designed to per- higher frequencies with increase of applied pressure 共the
form simultaneous normal and angular acquisition of resonance minima positions and its depth clearly identify the
reflected signals as the system is subjected to increasing or shift of the spectrum兲. The frequency minimum shift is about
decreasing controlled levels of loading. 0.4 MHz between 10 and 24 MPa. The shift of the frequency
In the experiments, a 0.77-mm-thick round plate with minima on pressure is similar in all pressure ranges, indicat-
25.4 mm diameter is mechanically loaded between the upper ing that the saturation point 共frequency independence兲 was
aluminum block A and the lower aluminum cylinder B. The not reached.

J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties 1429

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FIG. 7. Experimental reflection spectra 共amplitudes
versus frequency兲 for an aluminum/aluminum/
aluminum system under different pressure: 共a兲 normal
and 共b兲 angular incidence reflected spectra 共38-deg in-
cident angle兲.

The experimental results for oblique incidence of re- Ultrasonic data were collected using the dual-channel angle-
flected longitudinal waves are given in Fig. 7共b兲. Again, the beam contact scanning system described in Ref. 28. The nor-
spectra of the reflected signal shift to higher frequencies with mal and oblique reflected spectra from the adhesive bond
increase of pressure. The resonance minima at around 6 and were deconvolved with the reference signal as described in
12 MHz are clearly shifted together with the local minima Refs. 25 and 28. We continue the degradation process after
which appeared at approximately 9 and 10 MHz. The sensi- the measurements until the adhesive layer is easily separable
tivity of the minimum shift to pressure is slightly higher at from the substrates.
low frequencies than at high frequencies. Similar results At this stage the adhesive layer is removed from the
were obtained for a thin brass foil between Al substrates. joint and its bulk properties are measured again 共on a single
layer兲 to compare with the original ones which were mea-
B. Environmentally degraded adhesive joint sured after bonding but before degradation, using the recon-
struction method.24
The second set of validation experiments was performed
The adhesive joint samples were exposed to the environ-
on adhesive bonds with environmentally degraded interfacial
ment until moisture penetration was detected at one of the
properties. Adhesive joints were prepared with modified in-
interfaces by the 50-MHz focused transducer C-scan in the
terfacial properties and nominally constant bulk properties of
the adhesive layer. The reconstruction of properties was per- reflection mode 共at this frequency, the reflected signals from
formed from experimental data using the inverse model, the bottom and top of the adhesive layer are separated and
which includes transverse springs simulating poor contact the transducer is focused on the top interface兲. Figure 8共a兲
between substrates and an adhesive layer. The experimental shows a typical C-scan image obtained from a sample envi-
results were obtained for aluminum alloy bonded with com- ronmentally degraded for 73 h where the darker areas are
mercial FM-73 adhesive. Interfacial degradation was con- associated with water accumulation at the interfaces 共low
trolled by time in the environment of NaCl saturated solution reflection amplitudes indicating no disbond are bright areas兲.
at 68 °C. The sample preparation process was discussed in The image shows that the water-filled delamination is propa-
detail in Refs. 26 and 28. To isolate the interfacial degrada- gating inward from the edges. It is important to note the
tion from changes of bulk properties of the adhesive, alumi- C-scan image is related to one interface. We have performed
num adherents were prepared without anodization and prim- C-scans from both sides of the sample and found that the
ing, assuring fast interface degradation. In this case 100% C-scan images of both interfaces are statistically similar for
interface degradation occurs relatively fast 共in a few days兲. the type of environmental degradation performed in this

FIG. 8. 共a兲 C-scan of damaged area with 50-MHz focused transducer; 共b兲 reconstructed properties of transverse interfacial stiffness K T⬘ in the area marked by
dashed box in 共a兲.

1430 J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties

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plete disbonding. The obliquely reflected SV-wave spectra
show a significant shift 关Fig. 9共b兲兴 as one approaches the
edge of the scanned area. Therefore, the sensitivity of the
obliquely incident waves to the onset of such damage at the
interphase is stronger. This is in line with the model pro-
posed by Lavrentyev and Rokhlin20 to characterize adhesive
bond degradation due to moisture migration to the interface.
It accounts for formation of very thin water-filled interfacial
microdisbonds that produce very little effect on longitudinal
wave reflection at normal incidence. Such a hypothesis is
supported by the infrared measurements performed at
NIST,29 which show that the thickness of the typical water
layer diffused to the adhesive–adherent interface is below 40
nm. Such microdisbonds can be modeled by slip boundary
conditions 共zero stiffness transverse springs兲; however, the
bonded area contains arrays of small microdisbonds which
are modeled by finite transverse springs, which depend on
the total microdisbonded area.20

IV. INTERFACE AND LAYER PROPERTY


RECONSTRUCTION
The inverse algorithm was applied to reconstruct the set
of parameters 共3兲 and 共4兲 from the normal and oblique ex-
perimental spectra. For the Al/Al/Al system the imaginary
part of the complex interfacial spring corresponds to energy
loss due to ultrasonic scattering at the contact roughness on
the interfaces, and needs to be determined as a function of
FIG. 9. Spectra of the reflected signal at different positions in the environ- the nominal pressure together with other parameters. Attenu-
mentally degraded area of the adhesive bond. 共a兲 Normal incidence; 共b兲
ation in the aluminum layer is comparably low for both lon-
oblique incidence 关the curve labels are as in 共a兲兴.
gitudinal and transverse waves and is set to be zero during
reconstruction. As an example, Fig. 10 shows typical experi-
work. The 20- by 25-mm area, marked off by the dashed line mental 共points兲 and simulated 共lines兲 spectra after optimized
in Fig. 8共a兲, exhibits no visible damage in the C-scan image. matching of the spring model with the experimental spectra.
It was used for the dual beam 共normal and oblique兲 ultra- Solid lines represent the spectrum calculated from the recon-
sonic scan and property reconstruction. An image of the re- structed layer and interface properties, and the points are the
constructed transverse interfacial spring K T in this region is experimental data. The deviation between the experimental
shown in Fig. 8共b兲. Due to reverberation in the adhesive of and calculated spectra serves as an indication of the quality
the signal used for reconstruction, the K T image depends on of the reconstructed data. Both normal and oblique experi-
the reflection from both interfaces as was discussed in Sec. mental spectra are well represented by the calculated spec-
II B. trum for all features, including the local minima in the ob-
As an example, Fig. 9 shows normal and oblique inci- lique spectra.
dence reflection spectra for several points along the center- A summary of the reconstruction results of the bulk and
line x of the C-scan image in Fig. 9共a兲. The spectrum for the interfacial properties versus applied nominal pressure is
normal incidence 关Fig. 9共a兲兴 at these points is practically given in Fig. 11. The results show expected trends; for ex-
unaffected until x⫽20 mm, which is close to the disbonded ample, Fig. 11共a兲 demonstrates the increase of interfacial
area. The normal spectrum, however, changes as the scan normal and tangential springs with increasing pressure; how-
approaches the edge of the samples toward areas with com- ever, the damping shown in Fig. 11共b兲 decreases rapidly with

FIG. 10. Comparison between experimental and calcu-


lated reflection spectra for the aluminum/aluminum/
aluminum system. Calculations 共solid lines兲 were per-
formed using reconstructed spring constants: 共a兲 normal
incidence, and 共b兲 oblique incidence 共38-deg incident
angle兲.

J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties 1431

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FIG. 11. Reconstructed properties for an Al layer be-
tween Al substrates under dry contact as function of the
applied nominal pressure: 共a兲 interfacial stiffness K N⬘ ,
K T⬘ ; 共b兲 imaginary parts of the normal and transverse
interfacial springs 共damping兲; 共c兲 longitudinal and shear
velocities; and 共d兲 thickness of the aluminum layer ob-
tained. Dashed lines in 共c兲 and 共d兲 are properties deter-
mined on this thin aluminum layer by independent di-
rect measurements.

pressure. This is due to reduction of the interface scattering As discussed in Ref. 20, we can neglect viscous losses
with flattening of the asperities with pressure. The ratio due to water accumulation at the interface. Also, the interfa-
K T⬘ /K N⬘ for the data in Fig. 11共a兲 has a value between 0.42– cial microdisbonds are very small and flat; at these condi-
0.56. These values are reasonably close to those obtained in tions, in analogy with the results in Fig. 11共b兲 for the inter-
Refs. 9 and 23 共for extensive discussion of this ratio see Ref. facial damping on a rough interface at higher pressure, it is
23兲. Reconstructed aluminum foil properties—velocity and reasonable to assume that the interfacial scattering and ab-
thickness—do not change with the pressure. We performed sorption are very small and therefore we take the imaginary
direct measurements of the film thickness and shear and lon- part of the interfacial spring K T⬙ ⫽0. Attenuation in the adhe-
gitudinal velocities. Direct measurements are indicated in sive changes with degradation due to debonding of the knit
Figs. 11共c兲 and 共d兲 by dashed lines. They are in good agree- carrier fibers in the adhesive and ultrasonic scattering.30
ment with the reconstructed properties shown by solid and Therefore, the attenuation for shear and longitudinal waves
open points. in the adhesive is assumed unknown and to be reconstructed.
The bulk properties of the adhesive layer and the inter- Experimentally we observe two easily measurable resonance
facial properties between the layer and the substrates were
minima at oblique incidence 关Fig. 9共b兲兴; therefore, the K T
reconstructed from the experimental normal and oblique re-
effect is separable from the adhesive bulk properties, and the
flection spectra in the bonded area 20 by 25 mm marked by
interfacial transverse spring is reconstructed from the oblique
the dashed box in Fig. 8共a兲. As discussed in Sec. III B, the
spectrum.
normal reflectivity spectra Fig. 9共a兲 are not sensitive to small
An image of a reconstructed transverse interfacial spring
environmental degradation, while the minima position for
the angle beam spectra 关Fig. 9共b兲兴 exhibit significant shift. K T⬘ is shown in Fig. 8共b兲. High values of K T⬘ are shown by
This is consistent with the model of water-filled microdis- white and low values by dark gray levels. Significant inho-
bonds at the interface20 共tens of nanometers thick disbonds兲. mogeneity is observed in the image with transition from high
We take in the reconstruction the normal spring K N ⫽⬁ 共con- to low spring area. This contrasts with the C-scan image Fig.
tinuity of normal stresses and displacements兲 while keeping 8共a兲, which exhibits no changes in the same area. The tran-
the K T spring as unknown. There are two reasons for this sition zone in Fig. 8共b兲 appears ‘‘mushy’’ with highly vari-
decision: 共1兲 Due to low sensitivity of the experimental nor- able transverse springs; this supports the water-filled micro-
mal spectrum minimum to degradation, the reconstruction of disbond model20 共black points are noise兲. The ultrasonic
K N⬘ from these data is very susceptible to data scatter. 共2兲 beam has about 5 mm diameter and thus averaged properties
Due to limited transducer bandwidth, we can easily observe are measured in this area.
experimentally two minima for the oblique incidence in the The reconstructed data at the centerline 共at y⫽0) in the
reflection spectra at adhesive bond and only one minimum reconstruction area are shown in Fig. 12. The bulk properties
for the normal incidence 关Figs. 9共a兲 and 共b兲兴. As it was dis- 共bulk and shear modulus, longitudinal and shear ultrasonic
cussed in Sec. II B, from only one spectral minimum we attenuation, density and thickness兲 did not show change with
cannot separate the longitudinal modulus of the adhesive distance. This is expected since the samples stayed in the
from the normal K N interfacial spring. environment for only a few days. The interfacial transverse

1432 J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties

Redistribution subject to ASA license or copyright; see http://acousticalsociety.org/content/terms. Download to IP: 130.102.42.98 On: Sat, 22 Nov 2014 05:04:29
FIG. 12. Scan line of reconstructed properties of envi-
ronmentally degraded adhesive bond: 共a兲 transverse in-
terfacial stiffness 关horizontal solid line indicates the up-
per threshold level of the sensitivity to the K T⬘
reconstruction; the region from the left of the ‘‘1’’ ver-
tical dashed line correspond to the ‘‘good bond,’’ region
between the lines ‘‘1’’ and ‘‘2’’ corresponds to the
mushy area in Fig. 8共b兲兴; 共b兲 thickness; 共c兲 longitudinal
modulus (␭⫹2 ␮ ); 共d兲 shear modulus 共␮兲 of the adhe-
sive layer. The horizontal dashed lines in 共b兲, 共c兲, and
共d兲 indicate the trend of properties variation with dis-
tance.

stiffness K T⬘ 关Fig. 12共a兲兴 shows a significant decrease as the or the imaginary parts of the interfacial springs, which ac-
position approaches the right edge. Note that in this range K T⬘ count for the wave scattering at the interface, are determined.
has a similar order of magnitude as that for the dry contact In the reconstruction algorithm, the properties are combined
interface 关Fig. 11共a兲兴. In the line scan of the reconstructed K T⬘ in the form of eight nondimensional parameters, which are
shown in Fig. 12共a兲, we should distinguish three regions: 共1兲 determined from reflection spectra at two incident angles:
The left region from the vertical dashed line ‘‘1’’ corresponds normal and oblique.
to the ‘‘good bond’’ 共in the good bond area we cannot recon- It was shown that the layer bulk and interface properties
struct the interface anomalies by this method in the 5–15- could be separated if several resonance minima in the reflec-
MHz frequency range兲. In this range the value of the spring tion spectra are measured. If only one of such minima is
is between the threshold level of the spring reconstruction recorded in both normal and oblique spectra, only effective
sensitivity and K T⬘ ⫽⬁, which corresponds to the perfect properties of the layer can be reconstructed 共those include
共welded兲 boundary conditions between the adhesive and the combinations of layer bulk and interfacial properties兲. It was
substrates. The threshold level (K T⬘ ⬇3 * 1015 N/m3 ) was as- found that the attenuation in the layer and imaginary parts of
sessed by the sensitivity simulation 关see also Ref. 20 and Fig. the spring constants cannot be decoupled. It is suggested to
2共b兲兴. At K T⬘ above the threshold level the ultrasonic reflec- select only two attenuation variables as unknown while the
tion signature does not depend on the spring value. At K T⬘ other two should be considered constant during reconstruc-
below the threshold level, frequency minimum shift is de- tion.
tectable with its decrease. Therefore, we depicted the recon- The algorithm was validated by specially designed ex-
structed values of the good bond spring constant to be at this periments where layer properties were measured indepen-
upper threshold level of the sensitivity 共this shows some con- dently for comparison with the reconstructed values. One of
tinuity of the experimental data; however, it does not imply the experiments is done on an aluminum foil in dry contact
that the actual spring constants are measured and have these between two aluminum substrates. The attenuation in the foil
values兲. 共2兲 The middle transition region 共between the verti- was taken to be zero while the imaginary parts in the inter-
cal lines兲 corresponds to the mushy area in Fig. 8共b兲; it is facial springs were considered unknown. All eight param-
smoothed by the finite size of the transducer beam 共unsharp- eters were reconstructed. The reconstructed layer properties
ness effect兲. 共3兲 From the right of the vertical dashed line were found to be in good agreement with Al foil properties.
‘‘2’’ the bond is degraded. Also, the interfacial spring ratio K T⬘ /K N⬘ was found to be
close to that in the literature.9,23 The second experiment was
for environmentally degraded adhesive bonds prepared such
V. SUMMARY AND CONCLUSIONS
that mainly interface properties were modified. The longitu-
A method for determination of the set of acoustical, geo- dinal spectra were found to be weakly dependent on mea-
metrical, and interfacial properties of an isotropic layer em- sured position in the slightly damaged bonded area, while the
bedded between two known substrates was developed. The oblique spectra varied significantly. Thus, for reconstruction
properties include the layer density, elastic moduli, thickness, the longitudinal spring was set infinite and K T was assumed
and interfacial normal and transverse spring constants. Also, to be unknown and to be determined from experiment. For
either longitudinal and shear wave attenuations in the layer this case the attenuation in the adhesive layer was assumed

J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties 1433

Redistribution subject to ASA license or copyright; see http://acousticalsociety.org/content/terms. Download to IP: 130.102.42.98 On: Sat, 22 Nov 2014 05:04:29
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1434 J. Acoust. Soc. Am., Vol. 114, No. 3, September 2003 Baltazar et al.: Reconstruction of interface and layer properties

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