Experimental Mechanics (2013) 53:1017–1024
DOI 10.1007/s11340-012-9702-5
Out-of-Plane CTE Measurement Method
for Freestanding Thin Films
A.E. Mag-isa & S.-M. Kim & J.-H. Kim & H.-J. Lee &
C.-S. Oh
Received: 10 August 2012 / Accepted: 3 December 2012 / Published online: 14 December 2012
# Society for Experimental Mechanics 2012
Abstract An out-of-plane linear coefficient of thermal ex-
pansion (CTE) measurement method was developed to over-
come the difficulty in measuring the in-plane deformation of
freestanding thin films with a thickness of less than 1 μm. The
out-of-plane profile measurement was relatively easy with the
added advantage of simplicity, easy specimen preparation, and
a simple test setup. White light interferometry was used for
determining the out-of-plane thermal deformation as a func-
tion of temperature. Two types of supporting substrates, sili-
con and ZERODUR®, were used to account for the substrate
effect on the CTE measurement. Attempts were made to fit the
measured profiles using several peak functions and then find
the optimal one. The test procedures were demonstrated using
a freestanding 530-nm-thick aluminum film that was used in a
previous in-plane measurement method. The calculated CTE
value of this aluminum film was 23.7 ppm/°C, which was in
good agreement with the in-plane measurement result. The
out-of-plane CTE measurement method incorporating a zero
CTE substrate was shown to be the most convenient and
straightforward method.
Keywords Aluminum . CTE . Freestanding . Thin films .
White light interferometry . ZERODUR®
A.E. Mag-isa
Department of Mechanical Engineering, Kumoh National Institute
of Technology, Gumi, Republic of Korea
S.-M. Kim : J.-H. Kim : H.-J. Lee
Department of Nanomechanics, Korea Institute of Machinery
and Materials, Daejeon, Republic of Korea
C.-S. Oh
Department of Mechanical System Engineering, Kumoh National
Institute of Technology, Gumi, Republic of Korea
C.-S. Oh (*)
61 Daehak-ro,
Gumi, Gyeongbuk, 730-701, Republic of Korea
e-mail: ocs@kumoh.ac.kr
Introduction
Thin films are unarguably key components of modern
microelectronics [1] and major constituents in most micro-
electromechanical system (MEMS) devices. These films
are commonly applied in metallization and as intercon-
nects in the semiconductor industry [2] and as structural
elements in MEMS devices. For example, 0.2~2.5-μm-
thick aluminum films are used in complex interconnects
on ultra-large scale integrated circuits [3]. MEMS struc-
tures relying on thermal actuation take advantage of a large
coefficient of thermal expansion (CTE) for their operation
[4]. Bimaterial microcantilevers, which are often used for
microelectronic switching and actuation such as in the
microgripper reported in [5], are an example of the many
cases where a large CTE difference is desirable. However,
although a CTE difference is useful in some microstruc-
tures, it can also be detrimental to the proper operation and
reliability of MEMS devices and integrated circuits. The
thermo-mechanical stress resulting from a CTE difference
between the layers (dielectric, semiconductor, conductor,
and so on) in an IC stack or MEMS device affects the
device performance [3]. Furthermore, because heating and
cooling cycles are inherent to device fabrication, as well as
device operation, failures due to stress voiding and hillock-
ing are common [6]. To fully take into account the contri-
bution or effect of thermal expansion on the device
operation and performance, an accurate measurement of
its value should be made based on the same material, scale
size, and fabrication process that were used to manufacture
the devices.
Although a review paper [7] and standard test methods [8,
9] are available for the CTE measurement of bulk materials,
the complexity of handling fragile and very small specimens,
coupled with the difficulty of implementing measurements,
render most of these methods inappropriate for thin films.
Some specialized methods have been developed by numerous
1018
researchers to determine accurate CTE values for thin films.
Generally, the existing CTE measurement methods for thin
films can be categorized into two types based on the orienta-
tion used to allow and measure the deformation caused by
changes in temperature, i.e., in-plane methods and out-of-
plane methods.
In-plane methods are common, reliable, and applicable to
the CTE measurement of a film with a thickness as small as
approximately 1 μm. The microgauge fabricated on-chip
[10], digital image correlation [11–13], X-ray diffraction
[14–16], and interferometric strain displacement gauge
[17–19] techniques are examples of the methods in this
category. Unfortunately, the specimens and test apparatus
for such tests are difficult to prepare and set up. Moreover,
some of the methods [17–19] in this category require the
application of a constant load in the direction of the defor-
mation to keep the film taut and flat, thus eliminating any
out-of-plane deformation. This makes the specimen suscep-
tible to creep during a test.
On the other hand, the out-of-plane methods are fairly
straightforward and simpler to implement. However, they
rely on the carrier substrate or constituent layer (in the case
of bilayer specimens), and the CTE values are obtained
indirectly. The methods included in this category are the
wafer or substrate curvature method [20, 21] and bimetal
micro-cantilever method [22]. In most out-of-plane test
methods, the carrier or supporting substrate can affect the
measurement results.
To alleviate the difficulty in handling a micro-sized spec-
imen with a nanosized thickness, a simple yet effective
method was developed that will allow a straightforward
approach to obtain the linear CTE value of the thin film
under consideration. Likewise, it was made clear that the
Fig. 1 (a) (100) Si die (10×
10 mm) containing 5 freestand-
ing Al films (530-nm-thick and
500-μm-wide) fabricated using
MEMS processes. One of them
was extracted and transferred
onto (b) the Si or (c) the
ZERODUR® substrates
having a gap
Exp Mech (2013) 53:1017–1024
effect of the supporting substrate should be eliminated with-
out sacrificing the integrity of the measurement data. By
using a special substrate with a zero or almost negligible
CTE, this particular problem was dealt with instantly. The
test procedures proposed in this paper were demonstrated
and proved using a freestanding 530-nm-thick aluminum
film used in a previous in-plane measurement method [19].
Experimental Procedure
Specimen Preparation
The 530-nm-thick sputtered aluminum specimens previously
used for in-plane CTE measurements [19] were used again in
this paper for demonstration and comparison purposes. The
specimens were fabricated through a series of sputtering dep-
ositions, photolithographies, and finally bulk etching from the
backside of a (100) Si wafer, which had the shape shown in
Fig. 1(a). The 500-μm-wide and 2.5-mm-long freestanding
straight portions shown in Fig. 1(a) were removed from the die
and transferred to two different substrates, silicon and
ZERODUR®. The former was used as a supporting substrate
because silicon is one of the most frequently used materials in
the semiconductor and MEMS industries, and a wealth of
information on its CTE value can easily be found in the
literature. The silicon-supported film was used to demonstrate
the effect of the substrate on the measured CTE. ZERODUR®
is a special glass substrate with a zero or almost negligible
CTE value manufactured by Schott GmbH. This particular
substrate was the main carrier for the CTE measurement
method developed in this work. There were 540-μm and
600-μm gaps in the middle of a Si and ZERODUR®
(b)
(a) (c)
Exp Mech (2013) 53:1017–1024 1019

substrates so that the specimens could be made freestanding
when transferred onto them, and their surfaces were polished
using chemical-mechanical polishing for better surface con-
tact when the aluminum film was transferred. Prior to trans-
ferring the aluminum films, they were cleaned using O2
plasma to provide a better surface condition for holding the
film in place. The thin films were transferred to the substrates
by allowing them to float freely on deionized (DI) water,
which also contained the substrates. Sufficient time was pro-
vided so that the substrate, water, and film were at the same
temperature before the subsequent transfer was made.
Afterward, each film was scooped using a substrate and
positioned on top of the gap. The DI water helped to position
the film on the substrate and to prevent air trapping between
the film and substrate during transfer and so prevented the film
from delaminating as it underwent thermal expansion during
heating. The DI water is to the film on the substrate what
humidity is to a suction cup on a surface. The prepared Al
films on the Si and ZERODUR® substrates are shown in
Fig. 1(b) and (c), respectively. The films were aligned
perpendicular to the gap with the aid of the two holes in each
substrate, although the alignment didn’t affect the results at all.
Specimen Heating
The specimens were seated and heated in a small furnace
(Linkam’s THMSE 600) with a transparent quartz window.
An image of the entire furnace and its enlarged view focus-
ing on the ZERODUR® substrate holding an Al film are
shown in Fig. 2(a) and (b). The necessary temperature
profile as shown in Fig. 2(c) was provided and controlled
by using a controller (Linkham’s TMS 94), which was
capable of controlling the furnace temperature with a stabil-
ity of 0.1 °C. Each specimen was heated at a rate of 1 °C/
min up to the desired temperature and then held there for
5 min to allow thermal equilibrium to be attained prior to the
measurement. The low heating rate was necessary to ensure
that the specimen, supporting substrate, and furnace cham-
ber could achieve thermal equilibrium in the least amount of
time. Starting from room temperature, the specimen was

Fig. 2 (a) Compact furnace

(L×W×H0137×92×22 mm3)
with a quartz window for the
WLIM measurement, (b) its
enlarged view focusing on the
ZERODUR® substrate holding
an Al film, and (c) temperature
profile for a complete test

(a) (b)

100

80
[
Temperature, T [oC

WLIM
Scanning Pt. (< 10 s)

60 T1+5

1 oC/min

40 T1
t1 t1+5 t1+10

Loading Unloading
20
0 50 100 150 200 250 300
Time, t [min]
(c)
1020
heated up to 100 °C with measurements taken at 5 °C
intervals.
Out-of-Plane Thermal Deformation Measurement
During heating, only the freestanding part of the film over the
gap expanded freely because it was constrained at both ends
on the substrate. The resulting deformation took place out of
plane if a film was buckled initially. Thus, a white light
interferometric microscope (WLIM; Polytec’s MSA-400)
was employed over the area of interest (AOI) to acquire the
deformation profile (topography) of the specimen at each
temperature increment during the entire heating process. The
WLIM has an independent sub-nm out-of-plane resolution but
a variable in-plane resolution depending on the magnification
of the objective lens. For the size of the specimen at hand, a 5×
Michelson interferometric objective lens was sufficient to
fully cover the AOI (1×0.6 mm2). In this case, the lateral
resolution was 1.29 μm. Measurements were also made while
the specimen was cooled down from 100 °C to room temper-
ature (which is referred to as unloading throughout this paper)
in order to only check the effect of hysteresis on the measure-
ment result. The measurements were repeated multiple times
for each temperature to check the repeatability and verify the
thermal equilibrium during the test. It took about 10 s to scan a
specimen at a specific temperature. The topography or surface
profile data of a specimen at a pre-set temperature were
exported for the curve fitting. The measurement apparatus
Fig. 3 Out-of-plane CTE mea-
surement apparatus and schema-
tic diagrams illustrating setting
up of a specimen and curve
fitting
WLIM
6 DOF Stage
Furnace
Exp Mech (2013) 53:1017–1024
and schematic diagrams are presented in Fig. 3 to show the
constituents of an actual test setup and an overview of the key
test procedures such as heating and curve fitting.
CTE Calculation
In principle, the deformation profile should follow a trigo-
nometric sine or cosine function because the deformation
resulted from the buckling of a film fixed at both ends.
However, these functions could not be used to fit the measured
data because they are periodic in nature, whereas the data have
flat ends on both tail portions because the specimen was fixed
to the substrate. Thus, numerous peak equations, including
statistical probability density functions, were tried to fit the
data based on the least squares method. The beta, log-normal,
and Weibull distribution curves could describe the data per-
fectly, with few differences among their descriptions. The six-
parameter (a, b, c, d, e, f) beta function shown in equation (1)
was adopted for the curve fitting of all the deformation profiles
[23]. h(x) represents the out-of-plane height as a function of
the in-plane coordinate of x. This function can represent
symmetric as well as asymmetric shapes.


xcþdm e1 ð1 d Þ
xcþdm f 1
hðxÞ ¼ a þ b d me1 nf 1 ð1Þ
f 1
m ¼ eþf 2 ; n ¼ eþf 2
e1
After fitting the deformation profile to the corresponding
fitting function, the length of the fitted curve was computed
5x Michelson
Lens
Surface Profile
Temp.
Controller
Film on Substrate Curve Fitting
Hot Plate
Exp Mech (2013) 53:1017–1024
by line-integrating the function over the entire length of the
film. The initial length (L0) at a reference temperature (usu-
ally room temperature) and successive lengths (LT) at dif-
ferent temperatures for a specimen could be calculated using
the measured profiles. Thermal deformation (δT) is the dif-
ference between LT and L0. The thermal strain (εT) was
calculated by dividing the deformation by the initial length
using equation (2). The average linear CTE of a film (αav)
can be calculated using equation (3) by calculating the slope
of the thermal strain versus temperature plot.
dT L T  L0
"T ¼ ¼ ð2Þ
L0 L0
Δ"T
aav ¼ ð3Þ
ΔT
Results and Discussion
The successive shape changes of a film were measured (at
5 °C intervals) using the WLIM, as it underwent thermal
expansion when heated from room temperature to 100 °C;
the results are presented in Fig. 4. The specimens were
designated as S1 to S6 for the Si substrate and Z1 to Z6
Fig. 4 Successive shape changes of a specimen (Z6) on ZERODUR® substrate when heated from 30 °C to 100 °C (at 5 intervals)
1021
for the ZERODUR® substrate as shown in Table 1. It can
clearly be seen that the height increases as the temperature is
increased. In addition, it should be noted that there is no
delamination between the film and substrate because there is
no noticeable difference between the ends in any of the
profiles. One of the surface profiles was exported and fitted
with the beta function, as shown in Fig. 5. The fitted curve
was displaced above from the raw data on purpose to allow
a clear comparison between the two. It is evident that the
fitting function accurately follows the deformation, and this
was the case for most of the measurements. The square of
the correlation coefficient r2 was greater than 0.97 in every
case. The raw data and its fitted curve were overlapped and
inserted as an inset in the same graph. There was no notice-
able difference between the two.
Two types of deformation profiles were found during the
tests: a convex deformation outward from the gap, as shown
in Fig. 6(a), and a concave deformation into the gap, as
shown in Fig. 6(b). The deformation shape depends on the
amount of the trapped water in the gap of a substrate. If there
is enough DI water trapped in the gap, then its large capillary
force pulls down the film making it deform initially down-
ward. It is normally obtained naturally in the wet transfer
process. The convex shaped film tends to produce a more
continuous interferometer profile but sometimes prone to film
delamination while heating. However, there was negligible
1022 Exp Mech (2013) 53:1017–1024

Table 1 Summaries of CTE

values measured for Method & substrate Out-of-plane In-plane [19]
530 nm thick Al films
[unit: ppm/°C] Silicon ZERODUR®

Specimen Code CTE Code CTE

1 S1 19.1 Z1 24.9 Interferometric Strain/ Displacement

2 S2 18.9 Z2 22.0 Gauge (ISDG) method
3 S3 20.0 Z3 23.4
4 S4 21.3 Z4 23.5
5 S5 21.7 Z5 24.0
6 S6 21.6 Z6 24.1
Mean±S.D. 20.4±1.3 23.7±1.0 23.6±0.36

difference in the measured CTE value for either shape. All the CTE value from the in-plane measurements [19]. The mean
profiles were turned upside-down in case of concave defor- CTE (≈23.7 ppm/°C) of Al with the ZERODUR® substrate
mation. Figure 7(a) shows the thermal deformation profiles was almost identical to that (≈23.6 ppm/°C) obtained in the
from room temperature to 100 °C for a silicon substrate, in-plane result [19], whereas that (≈20.4 ppm/°C) with sili-
whereas Fig. 7(b) shows those for a ZERODUR® substrate. con was smaller than the reference value. It is evident that
In both cases, the films bulge consistently with an increase in the silicon substrate affected the CTE measurement of the
temperature. It can be seen that the height increment for the thin film because as the film expanded out-of-plane, the
ZERODUR® substrate is greater than that for the silicon substrate expanded in-plane, thus reducing the amount of
substrate. This indicates that the substrate had a significant vertical deformation for the film. This will translate into a
effect on the CTE measurement. The thermal strain versus smaller measured CTE value. It is interesting that the
temperature plots were obtained from the fitted curves of the amount of discrepancy (3.3 ppm/°C) was very similar to
corresponding profiles and shown in Fig. 8 for the two types
of substrates. The CTE values were obtained from the slope of
the trend lines of the plots. The data exhibits linear behavior,
which can be identified by the r2 of over 0.996, up to 100 °C.
It can be clearly seen that the CTE value (≈24.1 ppm/°C) with
the ZERODUR® substrate is higher than that (≈21.6 ppm/°C)
with the Si substrate.
Six replicate tests were carried out for each substrate, and
the CTE results are summarized in Table 1, along with the

25

Fitted Curve
Out-of-plane Height, h(x) [µm]

20

15 Raw Data

10 25
20
15

5 10
5
0
0 300 600 900
0
0 300 600 900
In-plane Coordinate, x [µm]
Fig. 6 Two types of deformation profiles during a CTE measurement:
Fig. 5 Raw height data measured by the WLIM and its fitted curve (a) convex deformation where the film deforms upward from the
using 6 parameters beta function (the inset shows the overlapped data substrate, and (b) concave deformation where the film deforms towards
with the fitted curve) the gap
 Exp Mech (2013) 53:1017–1024 1023

25 1800
Symbol Stage Fitted Line CTE [ppm/ oC]
Loading 21.3
[

1500
Out-of-plane Height, h(x) [µm

20 100 oC Unloading 20.8

[ppm
1200
Increasing Temp.

T
15
(5 or 10 oC

Thermal Strain,
intervals) 900

10
600

5
300
32 oC
Al Film (t = 530 nm)

0 0
20 40 60 80 100
0 200 400 600 800 o
In-plane Coordinate, x [µm] Temperature, T [ C]
(a) Fig. 9 Thermal strains showing little hysteresis and their
corresponding CTE values during the loading and the unloading stages
25 for an Al film on Si substrate (S4)
100 oC
[

the CTE of (100) silicon (3~3.5 ppm/°C) found in the

Out-of-plane Height, h(x) [µm

20
literature [24, 25]. In the case of the ZERODUR®-supported
Increasing Temp.
film, the circumstances presented above were no longer
15 (5 or 10 oC
intervals) present. Thus, we could directly obtain the CTE of the film
solely from the topography data. The CTE of ZERODUR®
10
is 0~10 ppb/°C [26], which is negligible compared with that
30 oC of the Al film. Accordingly, the CTE of a substrate should
5 be considered to obtain the true CTE of a specimen because
both experience the same amount of temperature change.
0
The substrate effect can be compensated by adding the CTE
0 200 400 600 800
of the substrate to the average CTE value from measure-
In-plane Coordinate, x [µm] ments. The CTE of the substrate should be measured by
(b) using a test standard [8, 9] if there is no certified CTE value
for the substrate. Therefore, the true CTE of a film (αtrue)
Fig. 7 Out-of-plane deformation of an Al film when heated from 30 °C can be calculated using equation (4) by adding the CTE of
to 100 °C for (a) silicon (S6) and (b) ZERODUR® (Z6) supported
the substrate (αS) to that of equation (3).
substrates
Δ"T
atrue ¼ aav þ aS ¼ þ aS ð4Þ
ΔT
1800 In addition, in order to check the effect of hysteresis on
Symbol Substrate Fitted Line CTE r2
Silicon 21.6 0.997 the measured value, a complete test following the full tem-
1500
ZERODUR 24.1 0.996 perature profile of Fig. 2(c) was performed for a specimen
[ppm

(S4) with Si substrate and shown in Fig. 9. The CTE value

1200
(≈20.8 ppm/°C) obtained in the unloading (or cooling) stage
T

21.6 ppm/ oC
Thermal Strain,

24.1 ppm/ oC was almost the same as that (≈21.3 ppm/°C) found during
900
loading (or heating). Henceforth, all the CTE values were
calculated based on the loading data only in order to reduce
600

300
Table 2 CTE values measured with two different objective lenses
Al Film (t = 530 nm)
0 Magnification of Lateral FOV CTE
20 40 60 80 100 objective lens resolution [μm] [mm × mm] [ppm/°C]
Temperature, T [oC]
5× 1.29 1.8×1.34 21.3
Fig. 8 Thermal strain versus temperature plots for Al films on silicon 10× 0.64 0.9×0.67 21.1
(S6) and ZERODUR® (Z6) substrates
1024
testing as well as processing time. Lastly, the effect of the
WLIM’s in-plane resolution on the CTE measurements was
investigated by comparing the results obtained using two
different objective lens (5× and 10×). The results are tabu-
lated in Table 2. It was found that the CTE measurement
was not sensitive to the in-plane resolution as long as the
field of view covered the area of the specimen under con-
sideration. The possibility of creep could be ignored
throughout the test because no load other than temperature
was applied, and the films were made to deform either
concavely or convexly initially (at room temperature),
which ensured that the film had no residual stress.
Conclusions
An out-of-plane CTE measurement method was developed to
alleviate the difficulty in measuring the in-plane deformation
of freestanding thin films with a thickness of less than 1 μm.
The test procedures were demonstrated using freestanding
530-nm-thick aluminum films used for the previous in-plane
measurement. It was found that the true linear CTE of a film
could be calculated by adding the CTE of the substrate and the
slope of the thermal strain versus temperature plot. The effect
of the substrate on the measured CTE could be eliminated by
using a special substrate with a zero or almost negligible CTE.
With its advantage of easy specimen preparation and test
setup, the out-of-plane CTE measurement method can be
adopted for the majority of thin films regardless of their
thickness. The measured CTE value of the aluminum film
was 23.7 ppm/°C, which is in good agreement with the
previous in-plane measurement result of 23.6 ppm/°C. The
out-of-plane CTE measurement method incorporating a zero
CTE or known CTE substrate was shown to be a convenient
and straightforward method and it can be applied to measure
the CTE values of ultra-thin films.
Acknowledgments This paper was supported by the Research Fund
of the Kumoh National Institute of Technology.
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