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15. Young modulus and Poisson ratio

measurements of TiO2 thin films deposited
with Atomic Layer Deposition

Article in Surface and Coatings Technology · January 2012

DOI: 10.1016/j.surfcoat.2011.10.050

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 Surface & Coatings Technology 206 (2012) 2459–2463

Contents lists available at SciVerse ScienceDirect

Surface & Coatings Technology

journal homepage: www.elsevier.com/locate/surfcoat

Young modulus and Poisson ratio measurements of TiO2 thin films deposited with
Atomic Layer Deposition
L. Borgese a, M. Gelfi a, E. Bontempi a,⁎, P. Goudeau b, G. Geandier c, D. Thiaudière d, L.E. Depero a
a
INSTM and Dipartimento di Ingegneria Meccanica ed Industriale, Università di Brescia, via Branze 38, 25123 Brescia, Italy
b
Laboratoire PHYMAT, UMR 6630, Université de Poitiers, CNRS SP2MI, Bd Marie et Pierre Curie, BP 30179, 86962 Chasseneuil, Futuroscope Cedex, France
c
LETAM – CNRS FRE 3143, Université de Metz ISGMP Bât. B Ile du Saulcy F-57012 METZ cedex, France
d
Synchroton Soleil Saint-Aubin, BP48 91192 Gif-sur-Yvette cedex, France

a r t i c l e i n f o a b s t r a c t

Article history: Atomic Layer Deposition (ALD) allows the deposition of thin films onto flat as well as complex geometry surfaces
Received 12 July 2011 with excellent conformality. Thicknesses of few atomic layers can be achieved. Moreover, low-temperature
Accepted in revised form 25 October 2011 deposition is possible and this enables the change of surface properties of many kinds of materials. Good
Available online 4 November 2011
adhesion characteristics and also good mechanical performance of ALD deposited thin films make the technique
extremely interesting for several applications, as for example micro-electronics.
Keywords:
ALD
TiO2 is a well studied semiconductor material because of its multifunctional properties that open a wide range of
TiO2 applications for example in photocatalysis, optics and solar cells. ALD is extremely completive to other technique,
Anatase to deposit titania thin films, employed even to improve the biocompatibility of many kind of materials.
XRD TiO2 thin films are deposited with ALD technique at low temperature (90 °C) onto Kapton substrate and then
Young modulus crystallized ex-situ after annealing at 300 °C. X-ray diffraction (XRD) techniques are very suitable for the analysis
Poisson ratio of structure and microstructure of films and surface layers. In this work, XRD in combination with in situ tensile
testing has been applied for the first time to measure elastic properties (elastic modulus and Poisson ratio) of
TiO2 anatase thin films obtained by ALD. For the experimental conditions, the tensile stage was installed
in a Synchrotron laboratory of Soleil. The information extracted from diffraction patterns is presented.
© 2011 Elsevier B.V. All rights reserved.

1. Introduction
Nanotechnology is a cross-sectional field of research that is
expected to trigger decisive breakthroughs in many industrial fields,
including energy, health, information and communication technologies
etc. Atomic Layer Deposition (ALD) is expected to play a major role in
the development of nanotechnology-related industrial applications
[1,2]. ALD is a self-limited growth method of thin films characterized
by the alternating exposure of the substrate to reactant vapors, resulting
in the sequential deposition of (sub)monolayers. It provides atomic
level control of thickness and composition, and is currently mainly
used in micro-electronics to grow films into structures with aspect
ratios up to 100/1 [3-5].
ALD has several advantages: the synthesis of a material can be
strictly controlled, by a stoichiometric point of view, the deposition
temperatures are relatively low (also less than 100 °C), the resulting
material is highly conformal, the repeatability is guaranteed and the
sample thickness versus deposition cycles is a linear function. Finally
⁎ Corresponding author.
E-mail address: elza.bontempi@ing.unibs.it (E. Bontempi).
the possibility to deposit onto almost all substrates (also organic)
opens a wide variety of application opportunities [6-12].
Among the materials that can be easily deposited by means of
ALD, titania is one of the most widespread. Titanium dioxide (TiO2)
has interesting applications in many research nanotechnologies fields
owing to its attractive physicochemical properties. Currently TiO2
thin films are employed in optics, as filters and anti-reflection coatings,
in catalysis as photosensitive layers and solar cells, in medicine, as
biocompatible coatings for biomaterials, and in electronics. Several
studies have been already performed on structural and microstructural
behavior of nano-sized titania, synthesized by different ways [13-15],
but detailed studies concerning ALD deposited TiO2 thin films are
lacking. In particular more comprehensive studies about their mechan-
ical properties are necessary for industrial applications. Indeed, despite
some theoretical works [16,17] about elastic properties of anatase,
experimental data are very few. Moreover the literature shows an
increasing interest in developing new experimental setups with the
required resolution and sensitivity for mechanical characterization of
nanostructures [18].
We have recently proposed the use of laboratory tensile testing to
measure elastic properties of TiO2 anatase films obtained by ALD [7], by
means of application of the DRAST method [19]. To minimise experi-
mental errors, high-2θ peaks are usually chosen. However, for thin

0257-8972/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2011.10.050
2460 L. Borgese et al. / Surface & Coatings Technology 206 (2012) 2459–2463

film, the scattering signal is too low to allow an accurate determination

of peak positions by means of laboratory equipment. The synchrotron
X-ray source reduces or eliminates many problems due to low intensity
and instrumental broadening also at high angles.
In the present work we propose a more comprehensive study about
elastic properties of anatase thin films obtained through ALD technique
after thermal annealing at 300 °C for several hours, performed with
Synchrotron radiation: we calculated elastic modulus and Poisson
ratio of a nontextured anatase thin film by studying the linear d-sin2ψ
curves as a function of the applied load (in dynamic conditions). In a
very recent work [20] we have studied the microstructure of similar
samples, to verify the possible presence of residual stresses (possibly
related to the phase transition from anatase to rutile), in static
conditions.

2. Material and methods Fig. 1. The tensile stress device placed at the centre of the goniometer into the XRD
measurement stage at Diffabs Beamline (Soleil).
Atomic layer deposition is performed in the Cambridge Nanotech Inc
Savannah 100 system. The reactor is a stainless steel cylinder (18.1 cm
diameter and 3.6 cm height) with a bottom heated plate of 179 cm2. method, with the only hypothesis being σ33 = 0 (where σij is the ij
Titanium oxide is deposited starting from tetrakis(dimethylamido)tita- component of the strain matrix). The diffraction peak position (2θhkl)
nium(IV) (TDMAT) as the titanium source and milliQ water (H2O) as change of an {hkl} plane family is studied as a function of the two
the oxygen source. TDMAT (99,999%) is purchased from Sigma Aldrich Euler angles ϕ and ψ defined in Fig. 2 [23]. Using X-ray diffraction, the
Chemical Co. (Germany) and used without any further purification. strain εϕψ measured in the direction eϕψ defined in the specimen coor-
MilliQ water is produced in laboratory with a Millipore DirectQ-5 dinates system (e11, e22, e33) by ϕ and ψ is given by Eq. (1).
purification system starting from tap water. The precursors are injected

 !
in the reactor directly from 25 g stainless steel reservoirs held respec- dϕψ sinθ0
tively the TDMAT at 80 °C and the H2O at room temperature to develop ε ϕψ ¼ ln ¼ ln ð1Þ
d0 sinθϕψ
enough vapour pressure. Nitrogen gas having 99,999% purity and a flux
of 20 sccm is used as the carrier gas to feed the precursors vapours alter-
natively to the reaction chamber. The deposition temperature is 90 °C In Eq. (1) dϕψ (d0) are the (unstrained) lattice plane spacing of the
and the base pressure of the reactor is 0.5 Torr. To avoid the precursor {hkl} planes and θϕψ (θ0) are the angular positions of the corresponding
condensation both valves and delivery lines are maintained at 120 ° C. diffraction peaks according to Bragg's law.
The carrier gas with unreacted precursors and reaction products are on the basis of linear isotropic elasticity theory, under the hypothesis
evacuated from the reactor through the exhaust by the rotary vane of in-plane stress the formula to express the relation between stress and
vacuum pump that also maintains the base pressure in the system. strain in the direction defined by the angles ϕ and ψ is Eq. (2)[24].
The processing cycle to deposit TiO2 thin films by ALD consists of a
  1  
0.1 s TDMAT pulse, 10 s purging time, a 0.1 s H2O pulse, and 10 of hkl 2 hkl
ln 1= sinθϕψ ¼ S2 σ ϕ sin ψ þ S2 ðσ 11 þ σ 22 Þ þ lnð1= sinθ0 Þ ð2Þ
purging time. The deposition rate is 0.0667 nm per cycle. TiO2 thin 2
films with a thickness of 200 nanometers are deposited onto Kapton
HN substrates 125 microns thick. Samples annealing was performed to In Eq. (2) S1hkl and ½ S2hkl are the crystallographic elastic constants
induce thin film crystallization. The samples are heated, with a ramp relative to the considered lattice planes {hkl}, σ11 and σ22 are normal
rate of 5 °C/min, in a Carbolite furnace (United Kingdom) at 300 °C for stress components and σϕ is the normal stress component in a direction
12 hours in air atmosphere. For structural and microstructural charac- defined by the angle ϕ.
terisation, XRD measurements are performed at Soleil Synchrotron, on When in-plane stresses are isotropic (σ = σ11 = σ22 = σϕ) Eq. (2)
the Diffabs beamline [21,22]. The diffraction diagrams are acquired in becomes Eq. (3).
reflection geometry. The selected energy is 8 keV and the beam size is
  1  
0.3 × 1 mm (vertical × horizontal). A conventional punctual detector is 2
ln 1= sinθψ ¼ S2 σ sin ψ þ 2S1 σ þ lnð1= sinθ0 Þ ð3Þ
used to scan the diffraction angle range between 24° and 90°. 2
A tensile stress device is placed directly at the centre of the goniom-
eter into the XRD measurement stage in Fig. 1. Five different loads are
applied to the sample and the corresponding XRD pattern is acquired. e33

3. Results and discussion

Ψ eΦΨ
Collected XRD spectra are processed with commercial TOPAS
software in order to accurately extract diffraction peaks position, inten-
sity, area and FWHM. The first parameter is necessary for the evaluation
of macro-stress [20] and the structure deformation due to an external ce e22
rfa
applied load. To evaluate elastic properties of TiO2 thin films, a method su

based on the study of the peak shift, as a function of sin2ψ is employed m

en Φ
e ci
Sp
[23-25].
The method is based on the following principle: diffracting planes e11
are used as a strain gauge, and elastic strains are measured in one or
several directions of the diffraction vector. In the case of polycrystalline Fig. 2. Representation of the sample reference system, ψ is the angle between the normal
films, the whole strain tensor can be obtained thanks to the sin2ψ to the diffracting planes and the sample surface normal.
 L. Borgese et al. / Surface & Coatings Technology 206 (2012) 2459–2463 2461

Plotting ln(1/sinθψ) versus sin 2ψ, one can obtain a straight line The combination of P* and m* experimental data allows also the
whose slope is proportional to σ and the intercept allows the deter- determination of the Poisson ratio according to Eq. (11).
mination of the stress free lattice plane spacing d0.  

The sin2ψ method is also applied for the determination of the Poisson −m
υf ¼ ð11Þ
ratio and the Young modulus of thin films [26]. Combining XRD ðP  þ m Þ
measurements with in situ tensile stress it is possible to study the
evolution of the sin2ψ curves as a function of the applied load, which It was also demonstrated by Renault et al [26] that from the ab-
allows the experimental calculation of the elastic constants of the thin scissa sin 2ψ0f of the common intersection point of the sin 2ψ curves,
film material, assuming a macroscopically isotropic elastic behavior of the value of Poisson's ratio of the film νf can be calculated, knowing
both the substrate and the film. the Poisson's ratio value of the substrate νs, according to Eq. (12).
The tensile tester supporting the sample is placed at the center of the
2 f
goniometer so that the loading direction corresponds to the e11 sample sin ψ0
υf ¼  ð12Þ
axis (Fig. 2). The film is supposed to be perfectly adherent to the 1−υs 1− sin2 ψ0 f
substrate so that the applied strains εf11 and εs11 are equal (as well as
the transverse strains εf22 and εs22). The indexes refer respectively to: Fig. 3 reports XRD pattern of TiO2 thin film annealed at 300 °C for
f = film and s = substrate. 12 hours without any applied load. Large halos at about 27, 37 and
Assuming a uniaxial applied stress state (σ Af Af
22 = σ 33 = 0), the 42° in 2θ (indicated by arrows) originate from Kapton substrate.
f
stress σ 11 is related to the load F by Eq. (4). The polyimide molecules are highly ordered along the chain axes as
well as in the lateral direction and furthermore are highly oriented
Af F in the film plane [27], but the polymer is semicrystalline. High angles
σ 11 ¼ ! ð4Þ
ES diffraction peaks of the TiO2 crystalline phase in spite of the low di-
b ef þ eS mensions of this ceramic film, are well-defined.
Ef
The use of X-rays beam from a synchrotron source reduces or
eliminates many problems associated with instrumental broadening.
In Eq. (4) b is the sample width, ef and es respectively the film and
In addition, synchrotron provides a source of highly monochromatic
substrate thickness and Ef and Es the thin film and substrate Young
radiation with sufficient intensity to obtain a signal from very thin
modulus, and the index A refers to the applied (load).
films materials, also in high diffraction angles range.
Combining Eqs. (2) and (4) one obtains Eq. (5) for a given {hkl}
The annealing temperature is lower than the Kapton glass transition
family plane of thin film:
temperature (second order transition Tg between 360 °C and 410 °C
    [28]). Then we assumed that thermal annealing has no influence on
f 2 f
ln 1= sinθψ ¼ P 1 sin ψ þ m1 ð5Þ the substrate structure [7].
Fig. 4 reports the curves of ln(1/sinθ) as a function of sin 2ψ for dif-
In Eq. (5) P1fand m1fare expressed respectively by Eqs. (6) and (7). ferent applied loads for the (116) (a), (220) (b), and (004) (c) crystal-
lographic family planes. As expected there is a linear behaviour of ln
2   3 2 3
(sinθ) versus sin 2ψ curves. For the (004) crystallographic plane at
1 þ υf
 1 þ υf
F sin 2ψ = 0.8, there is a slight variation of the linear behaviour. This is
¼ 4 5 þ4 5σ 11
f rf
P1 ð6Þ
Es es þ Ef ef b Ef probably due to the measurements conditions (the investigated
inter-planar distances are quite perpendicular to the sample surface).
2 3

 " #   
We don't consider these points for the linear fitting of the curves of
−υf F υf this set of data. As described, we calculated P1f and m1f according to
¼ 4 5
f rf rf 2
m1 − σ 11 þ σ 22 þ ln 1= sin θ0 ð7Þ
Es es þ Ef ef b E f Eqs. (6) and (7), then we obtained P* and m* from the linear fitting
of all P1f and m1f, versus the applied forces, curves by using Eqs. (8)
and (9). We perform this procedure for every considered crystallo-
In Eqs. (6) and (7) νf is the thin film Poisson ratio for the chosen
graphic plane. Considering EKapton = 5.17 ± 0.03 GPa [29] as the
{hkl} family plane and the r index refers to residual.
Young Modulus of the substrate, we extracted the Young modulus
Plotting all the P1f values, calculated for each applied force, versus
of the thin film material from Eq. (10). Since anatase thin film does
the applied force F, we obtain a linear curve. Its slope P* is expressed
not show any preferred orientation, the thin film is quasi-isotropic,
by Eq. (8).
" #

 1 þ υf 1
P ¼ ð8Þ
Es es þ Ef ef b

Similarly the curve of all m1f, calculated for each applied force, ver-
sus F is linear. Its slope m* is expressed by Eq. (9).
2 3


 −υf 1
4
m ¼  5 : ð9Þ
Es es þ Ef ef b

Then one can deduce the Young modulus Ef of the thin film from
P* and m*, only knowing the substrate Young modulus Es by using
Eq. (10).

! 
1 1 Fig. 3. XRD pattern of samples treated for 12 h at 300 °C. Crystallographic reflections
Ef ¼ −Es es : ð10Þ corresponding to anatase are reported. The substrate contributions are indicated with
ef bðP  þ m Þ an arrow.
2462 L. Borgese et al. / Surface & Coatings Technology 206 (2012) 2459–2463

a The curves reported in Figs. 4a, b and c have a common intersection

(116) F=0.9 N point at sin2ψ = 0.2. This condition allows the determination of the
0.5672
F=2.8 N
Poisson ratio also by the “Intersection method” proposed by Renault
F=7.5 N
F=9.5 N
et al. [26]. Using the tabulated value of Kapton Poisson ratio (νKapton =
0.567
F=11.2 N 0.34 [28]) the Poisson ratio of anatase thin film results νf = 0.27, in
0.5668 agreement with our reported experimental value.
0.5666 From theoretical elastic constants values of anatase [17], it is possi-
ln (1/sin θ)

ble to evaluate its Poisson ratio and Young modulus by means of

0.5664
Eqs. (13) and (14)[32].
0.5662
3B−2G
0.566 υ¼ ð13Þ
2ð3B þ GÞ
0.5658
9BG
0.5656 E¼ ð14Þ
3B þ G
0.5654
0 0.2 0.4 0.6 0.8 1
In Eqs. (13) and (14) B is the bulk modulus and G the shear modulus.
sin2ψ
The bulk modulus represents the resistance to volume change and is
b related to the overall atomic binding properties in a material, while
the shear modulus G represents the resistance to plastic deformation.
(220) F=0.9 N

0.5492
F=2.8 N Theoretical Poisson ratio, calculated by Eq. (13), results 0.35, and the
F=7.5 N elastic modulus, calculated by Eq. (14), results 157 GPa. We can
F=9.5 N
0.549 F=11.2 N
conclude that calculated Young modulus is in very good accord with
our experimental data.
0.5488 On the contrary, Poisson ratio is different form theoretical one
ln (1/sin θ)

(that appears to be very close to the theoretical rutile value of 0.26),

0.5486
but it is in accord with other data reported by Li et al. [33] and Shibata
0.5484 et al. [34].

0.5482 4. Conclusions

0.548
In this paper for the first time Synchrotron radiation X-ray diffrac-
0.5478
tion was performed in combination with in situ tensile stress mea-
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 surements to allow the determination of Young modulus and
sin 2ψ Poisson ratio of TiO2 anatase thin films grown by ALD at low temper-
ature. The conditions to apply the method are well fulfilled thanks to
c the very good adhesion characteristics of the thin films grown by ALD.
(004) F=0.9 N
The obtained experimental values of the Young modulus and Poisson
F=2.8 N
1.1235 F=7.5 N ratio of TiO2 anatase thin film are in agreement with experimental
F=9.5 N (and theoretical for E) literature data previously reported for TiO2
1.123 F=11.2 N anatase polycrystalline materials and thin films.

1.1225 5. Acknowledgements
ln (1/sin θ)

1.122 The authors are grateful to prof. Neil Zimmerman for useful discus-
sions about the paper structure. This project was partially financed by
1.1215 Galileo project 2007/2008 N°29. We must also thank Soleil, the French
synchrotron radiation facility (Saint Aubain, France) for providing
1.121 beam time through the program committee — Proposal N° 20080450
“Mechanical behaviour of thin ceramic layers deposited by ALD.”
1.1205
0 0.2 0.4 0.6 0.8 1
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