Marzyeh Moradi

Department of Materials Science

and Engineering,
Carnegie Mellon University,
5000 Forbes Avenue,
Roberts Engineering Hall,
Pittsburgh, PA 15213
Interface Characterization of
Man-Kwan Ng Al–Cu Microlaminates
Department of Mechanical Engineering,
Northwestern University,
2145 Sheridan Road,
Fabricated By Electrically
Evanston, IL 60208-3111
Assisted Roll Bonding
Taekyung Lee
Department of Mechanical Engineering, Interface characteristics of Al/Cu microlaminates fabricated by an electrically assisted
Northwestern University, roll bonding (EARB) process were studied to understand the underlying physical/chemi-
2145 Sheridan Road, cal phenomena that lead to bond strength enhancement when applying electrical current
Evanston, IL 60208-3111 during deformation. Peel tests were conducted for the Al/Cu roll-bonded laminates pro-
duced under 0 A, 50 A, and 150 A applied current. After peel tests using a microtensile
Jian Cao machine, the fractured surfaces of both the Al and Cu–sides were examined using scan-
Department of Mechanical Engineering, ning electron microscopy (SEM) for fractography and SEM-based energy dispersive
Northwestern University, (EDS) analysis. Results revealed the strong dependence of the fracture path and its mor-
2145 Sheridan Road, phology on the strength of the bond, which is influenced by various phenomena occurring
Evanston, IL 60208-3111 at the interface during EARB, such as microextrusion through surface microcracks, pos-
sible formation of intermetallic components and thermal softening during simultaneous
Yoosuf N. Picard1 application of strain and high current density. [DOI: 10.1115/1.4036149]
Department of Materials Science
and Engineering, Keywords: electrically assisted roll bonding (EARB), Al/Cu bilayer, joined interface
Carnegie Mellon University,
5000 Forbes Avenue,
Roberts Engineering Hall,
Pittsburgh, PA 15213
e-mail: yoosuf@andrew.cmu.edu

Introduction during EAMP in relation to process outcomes, e.g., surface finish,

flow behavior, microstructure evolution, etc.
Electrically assisted manufacturing processing (EAMP) utilizes
Electrically assisted manufacturing processing has many appli-
a continuous or pulsed electrical current in order to enhance the
cations in different industrial sectors such as aerospace, automo-
formability of a material undergoing deformation [1]. EAMP
tive and household appliances [1]. It has been recently shown that
offers many advantages such as a significant reduction in required
EAMP will improve the process performance of roll bonding
force and time, thus improving process efficiency [2]. EAMP can
microlaminates made of Al/Cu sheets [11]. Metallic laminates are
be used as an alternative method to conventional heat-assisted
composed of alternating layers of metals or alloys, often joined
metal forming processes where complicated, costly, and time
together at their interface by means of roll bonding processes
consuming steps of heating can be simplified in an efficient way
[12]. These laminates have shown great potential in a vast array of
just by applying electrical current to locally heat material under
industrial applications due to their unique properties such as light
deformation.
weight, improved corrosion resistance, higher fracture toughness,
Many attempts have been made to understand the role of
and better damping capacity [13–15].
electrical current in improving the plastic flow of material. Both
It has been shown that in addition to the less required force
thermal and athermal phenomena are attributed to EAMP [3–6].
during roll bonding, applying current will also enhance bonding
Heat generation and subsequent temperature increment in the
strength significantly [11]. However, comprehensive characteriza-
material due to the electrical current are known as thermal effects
tion of the bond interface incorporating the effects of initial
and are related to Joule heating [7,8]. Effects that arise from elec-
microstructure and applied current on the mechanical/microstruc-
troplasticity are known as athermal effects, where dislocation
tural response is still lacking. Such analysis should help to delin-
motion is accelerated through electron wind forces exerted by
eate the physical/chemical phenomena instigated by electrical
the applied current [9,10]. However, there is a lack of comprehen-
current.
sive and systematic studies revealing the intricacies related to fun-
Here, we implement the EARB process to fabricate Al/Cu
damental underlying mechanisms governing material behavior
microlaminates and then conduct peel test to evaluate the bonding
strength as a function of applied electrical current. The focus of
the present work is to thoroughly study the bond interface charac-
1
Corresponding author. teristics created during EARB. To achieve this, SEM-based EDS
Contributed by the Manufacturing Engineering Division of ASME for publication
in the JOURNAL OF MICRO- AND NANO-MANUFACTURING. Manuscript received
analysis and surface fractography of peeled surfaces were per-
September 16, 2016; final manuscript received March 1, 2017; published online formed after fracture on both the Al and Cu-sides. Coupling EDS
March 24, 2017. Assoc. Editor: Shiv G. Kapoor. with fractography analysis enabled us to explore the effects of

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 applied electrical current on accelerating the heat/electroplastic
(thermal/athermal) affected phenomena that govern bonding prop-
erties, e.g., intermetallic formation, material softening, microex-
trusion of subsurface material, etc. Thus, we can determine the
possible thermal/athermal effects of electrical current on the mate-
rial response particularly at the interface by studying the charac-
teristics of the interface.

Experimental Methods
A microrolling device was used to perform roll bonding
assisted by electrical current on commercially pure 1100 series Al
and C110 copper sheets having a 127 lm initial thickness in order
to fabricate micro Al/Cu laminates. This is a well-controlled pro-
cess, the details of which can be found in previous articles in
Ref. [11]. Roll bonding was performed in a plane strain condition
where the starting sheets are in the form of strips with approxi-
mately 10 mm width and several cm lengths [11]. Before roll
bonding, the surface of the sheets was prepared through cleaning/
degreasing steps by acetone followed by wire brushing. The afore-
mentioned steps were consistent for all specimens in this study
and are generally critical to enhancing roll bonding and improving
process performance [11]. Roll bonding was performed on the
sheets to obtain 50% thickness reduction. Figure 1(a) schemati-
cally illustrates the EARB process steps.
A special tactic was used to prevent thin sheet slippage during
roll bonding because of the small mass of inertia of the thin
sheets. The thin sheets were “clipped” together by a folded
stainless steel sheet, as shown in Fig. 1(b). Beside relative sheet
slippage prevention, the “clip” also made the sheet stack thicker
to achieve high thickness reduction, which was originally limited
by the machine roll gap setting limitation. The stainless steel clip
has a higher stiffness than that of Al and Cu, compression can be
transferred to the roll bonded materials effectively.
Fig. 2 (a) Schematic, showing illustration of the peel test of Al/
Cu roll bonded sheets being pulled by a microtensile machine
and (b) peeling force profiles of electrically assisted Al/Cu roll
bonded samples for 0 A, 50 A, and 150 A applied currents. Data
belong to the peel test of the roll bonded sheets by 50% thick-
ness reduction.
It must be noted that during EARB, electrical current was
passed through the sheets from the upper to the lower rolls. Here,
we examined the effects that arise by current application corre-
sponding to current levels of 0 A, 50 A, and 150 A [11]. To evalu-
ate the bonding strength for different levels of applied current
during roll bonding, peel tests were conducted on laminate com-
posites following the ASTM D1876T-Peel test, standardized for
small scale laminated sheets using a micro-uniaxial tensile
machine, schematically shown in Fig. 2(a). The peeling rate was
0.1 mm/s. More details of this experimentation can be found in
Ref. [11] of a previous study. Figure 2(b) shows the peeling force
profiles for roll bonded samples under the imposition of different
levels of electrical current.
Back-scattered electron detector (BSE)/EDS analysis and frac-
tography of Al and Cu peeled surfaces was performed using a
Quanta 600 SEM with 10 kV accelerating voltage and a 10 mm

Fig. 1 (a) Schematic of electrically assisted microroll bonding process of Al/Cu

sheets. The surface of the Al and Cu sheets is prepared by degreasing and wire brush-
ing before roll bonding and (b) a folded stainless steel “clips” thin sheets together.

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 Fig. 3 BSE/SEM images of the fractured surface of electrically assisted Al/Cu roll bonded sheets after the peel
test in low and high magnifications for: (a)–(c) Al-side and (d)–(f) Cu-side; produced under 0 A, 50 A, and 150 A
applied currents. Arrows refer to the features on the surface captured by BSE detector.
working distance. Surface roughness of Al/Cu sheets was meas-
ured using a Zygo three-dimensional optical surface profiler
before and after brushing.
Results and Discussion
Energy Dispersive Analysis of Peeled Al/Cu Fractured
Surfaces. Figure 3 shows the BSE imaging of the peeled surfaces
of laminates in both Al and Cu-sides for all three rolling conditions:
(0 A, 50 A, and 150 A applied current). It is seen that Cu on the Al-
side (Figs. 3(a)–3(c)) appears as circular shaped particles having
different sizes ranging from 5 to 20 lm. The Cu particles are fairly
well distributed on the surface (arrow in Fig. 3(b) as an example).
Morphological assessment indicates the Al sheet has a rough
surface indicative of ductile fracture (Figs. 3(a)–3(c), high magni-
fication BSE images). Ductile fractured surfaces typically appear
rough and irregular, consisting of many microvoids and dimples
[16] as indicated by the arrow in Fig. 3(b) as an example.
Figures 3(d)–3(f) show the fractography results for the Cu
sheet. BSE imaging shows evidence of Al presence on the Cu-side
where Al exhibits highly elongated morphologies and almost an
interconnected thin Al network (arrow in Fig. 3(d)). The Cu-side
surface is smoother than the Al-side (arrow in Fig. 3(d), high mag-
nification image). There are large Al regions (islands) of Al on the
surface (arrow in Fig. 3(e), high magnification image). The fine
Al-rich features seem to match the grain boundary morphology
(arrow in Fig. 3(f), high magnification image).
We note that the BSE imaging contrast can be attributed to
both differences in atomic composition (Z-contrast) as well as
surface topography. Hence, EDS analysis was performed to fur-
ther confirm Al/Cu-rich regions. Figure 4 shows EDS maps cor-
responding to the BSE images presented in Fig. 3 for both Al
and Cu-sides in low and high magnification images. Insets on the
right show the corresponding EDS maps for Al and Cu elements
separately. Maps of the Al-side surfaces (Figs. 4(a)–4(c)) indi-
cate a rough Al surface decorated with isolated Cu particles con-
sistent with BSE images (Fig. 3). EDS maps for Cu-side show
large Al regions as well as fine line features that are Al-rich as
was also observed by BSE in Fig. 3. This indicates that the
networklike features seen on the Cu-side surface by BSE are
indeed Al-rich.
Empirical observations using EDS analysis does not show a
significant variation in the morphology and distribution of Cu on
Al-side or Al on Cu-side for peeled surfaces, irrespective of
applied current during roll bonding. However, there is a consider-
able difference in the deformation behavior and mechanical
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response of Al/Cu sheets during roll bonding as well as peel test-
ing for different levels of the applied current [11].
Roll bonding on Al/Cu microsheets revealed a decreasing trend
for required force with increasing current; F150A < F50A ffi F0A
[11]. It was argued that this difference is related to heat generated
during rolling due to the plastic deformation and applied current
simultaneously. Temperature rise due to Joule heating can be
found based on equation: DT ¼ ððqE J 2 tÞ=ðqCp ÞÞ, where DT is the
adiabatic temperature rise, J is the current density, and t is the cur-
rent pulse duration. Here, qE , q, Cp are material parameters
including: electrical resistivity, density, and specific heat capacity
[17]. Current density, J, can be found by dividing the current
amplitude to the current passing area which is defined as the
roll-workpiece contact area. Contact area is dependent on the
workpiece thickness reduction which is 50%.
Herein, theoretical calculations of temperature rise also included
the heating effect of the stainless steel clip, treating the workpiece
as a composite material by considering the volume fraction of
each material. Theoretical estimation shows that the temperature
reaches around 350  C (623 K) for 150 A and close to 50  C
(323 K) for 50 A [11], assuming there is no heat loss during the
process. Significant temperature rise during roll bonding under
high current density should result in material softening and thus
reduction of required deformation force. This effect was not appa-
rent for a 50 A current condition where there was no observable
reduction in required force.
Additionally, recrystallization temperature is estimated to be
around 0.5 homologous temperature for pure Al and Cu; 193  C
(466 K) and 404  C (678 K), respectively. Therefore, in 150 A,
temperature is greater (Al) or equivalent (Cu) to the recrystalliza-
tion temperature. So, dynamic recrystallization and softening are
quite likely in the Al-side. High current-induced recrystallization
and softening should lead to: (1) larger thickness reduction; (2)
less required force; and (3) Cu/Al intermetallic components for-
mation at the interface. Higher resolution characterization by elec-
tron backscatter diffraction and transmission electron microscopy
are currently underway to clarify the expected consequences of
temperature rise in high current density (150 A case) in terms of
interdiffusive phenomena. However, thermal effects of the applied
electrical current in the form of microstructure/texture evolutions
or formation of strong intermetallic components will affect bond
interface properties such as bond strength, which is noticeable in
peel test results for 150 A case (Fig. 2(b)) showing a significantly
larger bonding strength compared to the other two experimental
conditions (50 A and 0 A).
For Al/Cu roll bonded with 50% thickness reduction, peeling
force increased with increasing applied current. Peeling forces are
SEPTEMBER 2017, Vol. 5 / 031001-3
 Fig. 4 EDS of the fractured surface of electrically assisted AI/Cu roll bonded sheets under
0 A, 50 A, and 150 A applied currents after the peel test in low and high magnifications for:
(a)–(c) Al-side and (d)–(f) Cu-side. Insets on the right show the corresponding EDS maps for Al
and Cu elements individually. Particle-shape features distributed on Cu and Al-sides belong to
the detected Al/Cu elements, respectively.

significantly larger for 150 A compared to 50 A and no current compared to Cu. For Al to preferable adhere to the Cu surface
(Fig. 2(b)). There is also a large fluctuation in the peeling force would also indicate that fracture occasionally preferred to choose
data for 150 A current (Fig. 2(b)). It seems that the predominant a path through Al rather than breaking the bond at the Al/Cu
effect of EARB magnifies the localized bond strength effect and interface.
causes fluctuations of the peeling force. However, the peeling
force could also be affected by the amount of abrasion during
sample preparation and its random nature could result in variation
in the amount, depth, and evenness of the scratches on the surface
before roll bonding.
To quantify this, roughness measurements were performed on
the Al and Cu sheets before and after brushing. Results of this
quantification (Fig. 5(a)) reveals a rougher surface created during
wire brushing on the surface of Al sheet compared with Cu sheet
having almost the same initial surface roughness. Because Al
is relatively soft compared with Cu [18], it is easier to produce
long/deep scratches on the surface by wire brushing. This will
have a significant effect on bonding enhancement during the roll
bonding of Al/Cu sheet [17,18]; the mechanism of bonding forma-
tion will be described later. The profile of the Al surface is shown
in Fig. 5(b). It shows a network of deep scratches/microcracks on
the Al surface as a result of wire brushing, which is consistent
with the morphology of the Al network seen on the Cu-side
(Figs. 3(d)–3(f)).
Knowing all these effects, quantitative analysis of the weight
percent of Al and Cu elements was performed on different regions
of peeled surfaces on both Al/Cu-sides from the low magnification
EDS maps (2  2 lm area). The average weight percent values
from this quantification with the standard deviation are shown in
Table 1. This was done to show a semiquantitative comparison of
the amounts of permanently attached metal after peeling for the Fig. 5 (a) Average of surface roughness measured for Al
and Cu sheets before and after brushing, indicating a higher
Al and Cu-sides.
value of roughness on Al sheet as compared with Cu sheet. (b)
Energy dispersive quantification indicates more Al on the Cu- Optical (left inset) of the Al surface after brushing showing an
side than Cu on Al-side. However, in case of 150 A, the weight interconnected network of scratches/cracks produced on the
percentages are very close. Higher percentage of Al on Cu-side surface of al sheets and corresponding roughness profile (right
can be explained in relation to the lower tensile strength of the Al inset) captured by Zygo surface optical profilometer.

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 Table 1 Variation of weight percent concentration of Al and Cu
elements by changing the applied current during roll bonding
Element Current (A) Weight percent (%) Standard deviation
Cu-side Al 0 6.9 1.1
50 4.5 2.5
150 2.9 0.8
Al-side Cu 0 2.5 2.1
50 0.9 0.3
150 2.1 0.8
This was extracted from the quantification of low-mag EDS maps of
peeled test samples for both Al/Cu-sides.
Based on the cumulative results of the EDS and fractography
analysis (Figs. 3 and 4), it is suggested that the fracture path dur-
ing peel tests is through different regions that we delineate
and denote as A, B, and C shown in Fig. 6(a). Region A is at the
Al/Cu interface where there can be a strong bond between two
sheets because of the extrusion of virgin metals through micro-
cracks, consistent with film theory [19]. It is argued that because
of the local hardening at the scratches created by wire-brushing,
microcracks are produced during rolling at the surface of the sheet
especially in the sharp regions, appearing darker in Fig. 5(b).
These regions promote the cracking of the top oxide layer due to
the stress concentration at the tip of scratches. This phenomenon
preferably happens on the Al-side surface because of greater oxide
formation on the Al-side and the brittle nature of aluminum oxide
[20]. Therefore, virgin metal from subsurface is extruded through
the microcracks and create metallurgical bond. During peeling,
these regions undergo necking and fracture, thus leaving a charac-
teristic vein pattern morphology on the surface.
Evidence of such patterns will be provided later in the fractog-
raphy of peeled surfaces section. Figure 6(b) schematically shows
the aforementioned mechanism and formation of metallurgical
bond created through interlocking of extruded materials from both
sides through microcracks during roll bonding. Figure 6(a), region
A could also be composed of unbounded areas where there is lim-
ited bonding between the two sheets and thus fracture would
Fig. 6 (a) Schematic of fracture path during the peel test at
the interface of Al and Cu roll bonded sheets. The suggested
path goes through different regions marked as A, B, and C in
the image corresponding to interface, Al-side and Cu-side,
respectively. (b) Schematic of the formation of metallurgical
bonds at the interface of roll bonded sheets produced by the
formation of chemical bonding between Al and Cu atoms
through the cracks created on the surface oxide layer during
rolling.
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choose this path. Region B denotes fracture through Al. The large
Al regions on the Cu sheet indicated preferential shear in the Al
(Figs. 3 and 4). This is plausible since Al is mechanically weaker
than Cu, and possibly weaker than the interface bond as well.
Region C denotes fracture through the Cu. Isolated Cu particles
on the Al sheet (Figs. 3 and 4) helps to suggest limited fracture in
the Cu. This also would suggest locally enhanced bond strength
exceeding the Cu strength, or perhaps localized Cu softening.
Based on results of quantification, shown in Table 1, it is found
that the weight percent of Al on Cu-side and Cu on Al-side is
larger for a 0 A current condition. This suggests a significantly
larger fracture path through both sides of the bond (Al, Cu sheets
regions B and C in Fig. 6(a)) rather than at the interface
(Fig. 6(a), region A). Dividing the weight percent of Al on Cu-
side to Cu on Al-side, we find that the ratio is 2.8, 5.0, and 1.4 for
0, 50, and 150 A, respectively. This suggests preferential fracture
through Al for 50 A and 0 A, but less so for 150 A. This could in
part explain why 150 A required lower peeling force (Fig. 2(b)).
Because the overall strength of Al is lower than Cu [18], more
fracture through Al-side requires a lower peeling force.
In 150 A, the fracture path is almost evenly distributed between
Al and Cu-sides (1.41) and so it chooses the alternate paths
between Al and Cu-sides or through the interface (region A,
Fig. 6(a)). Hence, it can be argued that the strength of material in
Al-side is also very high, so the fracture does not go through the
Al-side, presumably due to the formation of strong Cu-Al inter-
metallic components. It can also be suggested that at high current
density, because of the thermal effects and softening of material
particularly Al, they can more easily extrude through the fractured
regions of the oxide layer (Fig. 6(b), left inset) and provide a path
for interdiffusion of Cu and Al elements through the interface and
promote the formation of intermetallic components.
Fractography of Peeled Al/Cu Fractured Surfaces. Fractography
of peeled surfaces shows evidence of Cu particles (Fig. 7(a)),
deep valleys (Fig. 7(b)), and vein patterns (Fig. 7(c)) on the frac-
tured Al surfaces. The surface of the Al-side for 50 A is rougher
compared with the other two current conditions, showing elon-
gated deep valleys because of Al detachment from the Al-side
(Fig. 7(b)). This is in agreement with EDS quantitative results for
50 A (5.03, the ratio of Al on Cu-side to Cu on Al-side). In 150 A
case, the surface is smoother and shows more occurrences of the
vein pattern (Fig. 7(c)) indicative of greater localized heating.
Fractography for the Cu-side shows the presence of an Al elon-
gated network on the surface (Fig. 7(d)). Results show a smoother
surface as compared to the Al-side, particularly for 150 A
(Fig. 7(f)). They also show less vein pattern formation and evi-
dence of significant plastic flow on the Cu-side as compared to
the Al-side. The reason for this was explained previously, as the
roughening effects are more prominent on the Al-side during wire
brushing. Consequently, the stress concentration at the rough
regions of the Al-side promotes cracking of the oxide layer during
roll bonding. Since the Al oxide layer is more brittle [20] than the
Cu oxide layer which has a ductile nature [18], it undergoes more
cracking during roll bonding and allows fresh Al in the subsurface
to extrude through the microcracks. Fractography and observed
higher roughness for the Al-side compared to the Cu-side suggests
the fracture path prefers Al-side rather than Cu-side. Additionally,
more heat generation by applying more current softens the mate-
rial and eases plastic deformation as mentioned previously, which
may result in more material flow through microcracks and inter-
locking of materials at the interface.
This will lead to increase in the ductile fracture instead of
brittle fracture during peeling. Plastic flow through microcracks
creates bonding between two extruded materials from opposite
sides, leaving characteristic vein patterns on the fractured surface.
So, more observed vein patterning suggests more plastic deforma-
tion occurred during bonding. Hence, more vein patterns suggest
more ductile fracture.
SEPTEMBER 2017, Vol. 5 / 031001-5
 Fig. 7 Secondary electrons (SE) images of fractured surfaces observed for (a) 0 A, (b) 50 A, and (c) 150 A cur-
rents; in low and high (boxes) magnifications for: (a)–(c) Al-side and (e)–(f) Cu-side

Fig. 8 SE images of fractured surfaces observed for 0, 50, and 150 A currents for: (a) Al-side
and (b) Cu-side, showing the different types of features on the fractured surfaces indicated by
numbers 1–5. Number 1 refers to unbounded areas, 2 to the Al/Cu particles on the Cu/Al-sides,
3 to the area that vein patterns are created, 4 to the faceted regions caused by shear of Al or
Cu during detachment from their sides, and 5 to the regions that underwent brittle fracture
during peeling, leaving microcracks on the surface.

The presence of such vein patterns is greater in extent in the case
of 150 A (Fig. 7(c), high magnification image) than the two lower
current cases. Less vein pattern in Al-side for 0 A and 50 A shows
that the nature of fracture is more brittle at the interface during
peeling compared with 150 A. Five different types of morphologi-
cal features are designated for our fractography study. The first fea-
ture type is regions of unbounded area where there is no bond
created between two sheets during roll bonding. The second feature
type is large area attachments of Cu on Al-side or Al on Cu-side.
The third feature type is vein pattern. The fourth feature is
regions with faceted morphology indicative of local shear and
detachment of Cu from Cu-side and Al from Al-side. The last
feature type is microcracks or regions with rough surfaces that are
attributed to brittle fracture. All of these feature types are indi-
cated in Fig. 8 for Al/Cu-sides. The detachment of Al or Cu from
their side and sticking on the other side create valleys with
smooth, flat (facet) surfaces, characteristic of brittle fracture.
These valleys with flat surfaces are evidence of shear in Al and
Cu during peeling. It can be concluded that EARB Cu/Al fracture
is a combination of ductile and brittle modes in which the ductile
fracture occurs at the extruded material joints and leave ridges
and dimples on the surface. The brittle fracture occurs where there
is a strong interface bond, and cracks propagate through the sheets
rather than the interface to leave a faceted surface morphology.

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 Other areas are just unbounded regions. The fluctuation of peeling
force can also be related to this path (unbounded areas).
Conclusions
Electrically assisted roll bonding was performed on Al/Cu micro-
sheets to study the effects of the applied current on the process per-
formance as well as the mechanical properties of fabricated
laminates by conducting peeling tests and the subsequent fractured
surface characterization. From this study, it is concluded that the
thermal/athermal effects of current result in enhancing the bonding
strength by enhancing microextrusion of virgin subsurface material
through the cracks created on the surface of the sheets during roll
bonding. Thermal effects of high current density ease of plastic
flow by softening the material at the interface. It also increases the
interdiffusion of Al/Cu elements through the paths created during
cracking of oxide layer predominantly on the Al-side to likely form
intermetallic components that improve the influence of interface
strength on fracture mode. Evidence of the microextrusion mecha-
nism is in the form of vein patterns more prominently observed in
the 150 A condition, where there was enhanced bond strength.
Acknowledgment
The support from the National Science Foundation (CMMI
Grant No. 1463204) is gratefully acknowledged.
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