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Applied Surface Science 370 (2016) 306–311

Contents lists available at ScienceDirect

Applied Surface Science

j ournal homepage : www.elsevier .com/ locate /apsusc

Protection of brittle film against cracking

J. Musil ∗, J. Sklenka, R. ˇ Cerstvý

Department of Physics andNTIS—European Centre of Excellence, University of West Bohemia, Univerzitní 8, 30614 Plzeˇ n, Czech Republic

a r t i c l e i n f o

Article history:

Received 11 November 2015

Received in revised form 8 February 2016

Accepted 13 February 2016

Available online 16 February 2016

Keywords:

Zr Si O film

Mechanical properties

Transparency

Film cracking

Protective film

Magnetron sputtering

a b s t r a c t

This article reports on the protection of the brittle Zr Si O film against cracking in bending by the highly

elastic top film (over-layer). In experiments the Zr Si O films with different elemental composition and

structure were used. Both the brittle and highly elastic films were prepared by magnetron sputtering

using a dual magnetron. The brittle film easily cracks in bending. Onthe other hand, the highly elastic filmexhibits enhanced resistance to cracking in bending. Main characteristic parameters of both the brittle

and highly elastic films are given. Special attention is devoted to the effect of the structure (crystalline,

amorphous) of both the brittle and highly elastic top film onthe resistance of cracking of the brittle film.

It was found that (1) both the X-ray amorphous and crystalline brittle films easily crack in bending, (2)

the highly elastic film can have either X-ray amorphous or crystalline structure and (3) both the X-ray

amorphous and crystalline, highly elastic top films perfectly protect the brittle films against cracking in

bending. The structure, mechanical properties and optical transparency of the brittle and highly elastic

sputtered Zr Si O films are described in detail. At the end of this article, the principle of the low-

temperature formation of the highly elastic films is also explained.

© 2016 Elsevier B.V. All rights reserved.

1. Introduction

It is well known that brittle films very easily crack during bend-

ingwhen theyare depositedon the flexible substrates. The cracking

of thebrittle films is their serious drawbackbecause the crackscre-

ated in the film interrupt its function [1–12]. Therefore, it is vitally

important to prevent cracking of the brittle films.

Recently, it was reported that the brittle film can be pro-

tected against cracking by the elastic top film (protective film)

with the high hardness H ≈15 to 25GPa, low elastic modulus

E * =E /(1− 2) which results in a high ratio H /E * ≥0.1, high elastic

recovery W e≥60% and compressive macrostress ( < 0) [13–16];

here E is the Young’s modulus and is the Poisson’s ratio. In the

experiment described in Ref. [17] it was shown that the amor-

phous brittle film over-coated by the crystalline elastic film does

not cracks, i.e. the system of two layers – brittle bottomfilm/elastictop protective film – exhibits an enhanced resistance to cracking.

However, there is a questionif also thecrystalline brittle filmcanbe

protected against cracking by an elastic top film and if this elastic

top film can also have the X-ray amorphous structure. The investi-

gation of the effect of the structure of both the brittle film and the

∗ Corresponding author. Tel.: +420 377632201.

E-mail address: [email protected] (J. Musil).

elastic protective film on the resistance of cracking of the brittle

film is the main subject of this article.This article reports on the two-layer coatings composed of brit-

tle bottom film and top elastic film with different compositions of

crystallographic structure of both films: (a) a-+ c-, (b) c-+ c-, (c)

a-+a-, and (d) c-+ a-; here a- and c- denotes the film with amor-

phous andcrystallinestructure, respectively,see Fig. 1. Physicaland

mechanical properties, and optical transparency of individual films

(a- brittle, c- brittle, a- elastic and c- elastic) and couples of these

films (the bottom brittle film + the top elastic film) are reported in

detail.

2. Experimental details

The Zr Si O coatings with different physical and mechanicalproperties were deposited on the Si (10 0) substrate and the Mo

strip (60×10×0.1mm3) by reactive magnetron sputtering using

a dual magnetron equipped with Zr/Si targets of 50mm in diam-

eter composed of a circular Si (10 0) plate (∅ 38mm) fixed to the

magnetron cathode by Zr fixing ring with inner diameter ∅in. The

dual magnetron was operated in ac pulsed bipolar mode gener-

ated by a pulsed power supply DORA MSS-10 with a maximum

output power 10kW. The repetition frequency f r of pulses was

2 kHz and ac frequency of negative half-sinusoids inside pulses

was 112kHz. More details on the deposition system are given in

Ref. [17].

http://dx.doi.org/10.1016/j.apsusc.2016.02.132

0169-4332/© 2016 Elsevier B.V. All rightsreserved.

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J. Musil et al. / Applied Surface Science 370 (2016) 306–311 307

Fig. 1. Four two-layer coatings composed of brittle bottom film and top elas-

tic film with different combinations of the structure of bottom and top films.

(a) crystalline/amorphous couple, (b) crystalline/crystalline couple, (c) amor-

phous/amorphous coupleand (d) amorphous/crystalline couple.

The films were sputtered under the following conditions: dis-

charge current I da =1 A averaged over the pulse period T = 1/ f r ,

target power density Sd =P d/S≈25 W/cm2, substrate bias U s =U fl,

the substrate temperature T s =RT (the unheated substrate) and

500 ◦C, substrate-to-target distance ds−t =80mm, partial pressure

of oxygen pO2 = 0 and 0.15Pa for the brittle films and the elas-

tic films, respectively, and total pressure pT = pAr + pO2 = 1Pa;

here S is the whole area of the magnetron target and U fl is

the floating potential. At first, single layer coatings were sput-

tered on the Si (10 0) substrate, glass substrate and the Mo strip(60×10×0.1mm3), their physicaland mechanical propertieswere

measured and their resistance to cracking was assessed by bend-

ing of the coated Mo strip around a fixed cylinder. Physical and

mechanical properties of sputter deposited single layer films and

their elemental composition are given in Table 1. Then, two-layer

coatingswith differentcrystallographic structureof the bottom and

top films (layers) were sputtered. Their physical and mechanical

properties were also measured and their resistance to cracking was

also assessed by bending of the coated Mo strip, see Table 2. Both

films in two-layer coatings were sputtered without an exposure to

the air simply by changingthe partial pressure of oxygen pO2 in the

Ar+O2 sputtering gas mixture.

The structure of sputtered films was characterized by X-ray

diffraction using an XRD diffractometer PANalytical X’pert PROin Bragg-Brentano configuration with CuK radiation. The ele-

mental composition was determined by X-ray Fluorescence (XRF)

spectroscopy with PANalytical XRF Spectrometer MagiX PRO.

Mechanical properties of films were determined from load vs.

displacement curves measured by a microhardness tester Fisch-

erscope H100 with Vicker’s diamond indenter at a load L=20mN.

For all sputtered films the ratio d/h of diamond depth impression

d in the film and the film thickness h was less than 0.1. It indicates

Fig. 2. X-ray (XRD) diffraction patterns of brittle – amorphous (film 1) and crys-

t alline ( film 2) and e last ic – amo rphous (fi lm 3) an d crys tall in e ( film 4) Zr S i O

films with propertiessummarized in Table 1.

that the measured hardness H of sputtered films is not influenced

by the substrate [18,19]. The macrostress and the thickness h of

thefilms were measured usinga stylusprofilometerDEKTAK 8. Themacrostress was determined from the thickness h and curvature

of the films deposited on Si (10 0)strips (35×5×0.64mm3) using

a Stoney’s formula [20]. The resistance of the film to cracking was

tested by a bending test. The coating was deposited on a Mo strip

(80×10×0.1mm3) and the coated Mo strip was bended around a

fixed cylinder of diameter r up to the occurrence of cracks in the

coating surface. More details are given in Refs [13–16]. The trans-

parency of Zr Si O layerswas measured inthe range from 300 to

800nm using a spectrometer Specord M400.

3. Results and discussion

3.1. Mechanical properties and structure of Zr Si O films

Physical and mechanical properties of single-layer Zr Si O

films are summarized in Table 1. From this table it is seen that

(1) the amorphous and crystalline films can be (i) sputtered from

a composed Zr/Si target, see Fig. 2, and (ii) either brittle (eas-

ily crack) or highly elastic (resistant to cracking) films can be

formed, (2) the brittle crystalline and amorphous films exhibit a

low ratio H /E

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308 J. Musil et al. / Applied Surface Science 370 (2016) 306–311

Fig. 3. Surface morphology of one-layer brittle film (a) the amorphous film (thefilm No. 1) and (b) the crystalline film (the film No. 2) after bending of coated Mo

strip (the film/Mo strip couple) around cylinder of radius r =10mm. Physical and

mechanical properties of the film 1 and 2 are given in Table 1.

(3) the elastic amorphous and crystalline films resistant to cracking

exhibit a high ratio H /E * ≥0.1 and high elastic recovery W e >60%,

compressive macrostress ( < 0), high optical transparency in visi-

ble and IR regions and strongly differ in the content of Zr and Si, (4)

the elastic amorphous film is soft and contains more Si compared

withZr (Si/Zr> 1),(5)the elastic crystallinefilm is hard and contains

more Zrcompared with Si(Si/Zr < 0), (6)thebrittleandelasticamor-

phous films exhibit a low compressive macrostress ( < 0), (7) the

brittle crystalline films exhibit tensile macrostress ( >0) and low

hardnessH ≈14GPa, (8) the elastic crystalline films exhibit a com-

pressive macrostress ( < 0), relatively high hardness H ≈17GPa

and almost the same value of the effective Young’s modulus E * as

the brittle crystalline film. These properties are controlled by the

elemental composition of films and their deposition rate aD, i .e.by

the energy delivered to the film during its growth.

The combination of individual films (layers) in the two-layer

Zr Si O coating makes itpossible to find the effect of the crystal-

lographic structure and mechanical properties of the bottom and

top layer on its resistance to cracking in bending.

3.2. Resistance of two-layer coatings to cracking in bending

At first, the brittle amorphous (the film No. 1) and the brit-

tle crystalline (the film No. 2) films, i.e. the single-layer Zr Si O

films, deposited on Mo strip were bended around cylinder of

radius r =10mm. Both coatings cracked in bending due to lowratio

H /E * < 0.1 and low elastic recovery W e < 60%, see Fig. 3 and Table 1.

Cracks are perpendicular to the direction of bending. On the other

hand, the elastic amorphous (the film No. 3) and the elastic crys-

talline (the film No. 4) single-layer films deposited on Mo strip do

not crack and exhibit no cracks after bending around cylinder of

radius r = 10mmdue to highratioH /E * > 0.1 and high elastic recov-

ery W e >60%.

Then, both brittle films (the film Nos. 1 and 2) were overlapped

with the highly elastic top films exhibiting high ratio H /E * ≥0.1,

highelasticrecoveryW e > 60%and compressive macrostress (

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Fig. 5. Four combinations of the indentation curves of the bottom brittle film and the top elastic film which prevent cracking of the bottom brittle film: (a) the film 1+ the

film 4, (b) the film 2+ the film 4, (c) the film 1+ the film 3 and (d) the film 2+ the film 3. Indentation curvesweremeasured onthe filmssputtered on Si (10 0) substrates.

5. The bottom brittle film with the lower hardness than that of top

filmcan be protected against cracking by the harder topfilm. On

the other hand, the bottom brittle film with the higher hardness

than that of top film can be protected against cracking by the

softer top film.

3.4. Optical transparency

Very interesting is the optical transparency of individual films.

Therefore, the Zr Si O films were also sputtered on glass sub-

strates. The optical transparency was measured in a wide range of

wavelengths from250 to 800 nm. Results of these measurements

are given in Fig. 6. From this figure it is seen that while brittle films

(the film No. 1 and the film No. 2) are opaque, the elastic films are

well transparent. The opacity of the brittle films is due to a large

amount of free Si and Zr atoms in the film. The transparency of

the elastic film with higher content of Si is practically the same as

that of the glass without film and higher than that of the elastic

film with the higher content of Zr. This difference is due to the fact

that the Zr Si O film with higher Si content essentially representsan SiO2 film which almost completely eliminates reflections at the

film/glass substrate interface. This is a big advantage of the elastic

Zr Si O film withhigh Sicontent. Ontheotherhand,thedisadvan-

tage of this filmis itslow hardnessH ≈7 GPa. Onthe other hand, the

elastic Zr Si O film with higher Zr content is the ZrO2 based film

with lower optical transparency due to reflections at the film/glass

substrate interface but with a higher hardness H ≈17GPa.

4. Low-temperature sputtering of flexible nanocomposite

films

At present, there is an urgent need to master the forma-

tion of crystalline or at least nanocrystalline flexible films on

heat sensitive substrates such as polymer foils, textiles, plastics,

Fig. 6. Transmittance ofthe brittle Zr Si O films– amorphous (film 1)and crys-

talline(film2)andtheelasticZr Si O filmswith enhancedresistance tocracking –amorphous(film 3) andcrystalline (film4) sputteredon glasssubstrate as a function

of wavelength of the electromagnetic wave.

polycarbonates, etc., without the substrate heating. It is a very

difficult and vitally important task because the formation of the

flexible films withenhanced resistance to cracking at low substrate

temperatures T s≤100 ◦C is of a great potential for many advanced

applications, namely for the flexible electronics, flat panel displays,

micro-electromechanical (MEMS) systems, formation of the func-

tional films on polymer foils and fabrics, etc.

The formation of the flexible films on unheated substrates is

possible. It is basedon the replacement of the equilibrium substrate

heating (T s/T m) by the non-equilibrium atomic scale heating, i.e.

on the energy E p delivered to the growing film by condensing and

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310 J. Musil et al. / Applied Surface Science 370 (2016) 306–311

Fig. 7. Schematic illustration of two dimensional (2D) Thornton’s structural zone

model (SZM) extended into region of low-pressure sputtering. Adapted after Ref.

[22].

bombarding particles; here T m is the melting temperature of the

material of the film. The principle of formation of the flexible films

on unheated substratesis illustrated in Fig.7. This figure represents

the two dimensional (2D) structural zonemodel (SZM) of sputteredfilms developed by Thornton [21] extended to low sputtering gas

pressures p≤0.1Pa [22]. The zone T of the SZM represents dense,

voids-free films in compression ( < 0) with enhancedresistance to

cracking; here is the macrostress in the film.

From Fig. 7 it is clearly seen that just the zone T expands to low

values of the ratio T s/T m→0 with decreasing argon pressure pAr.

This means that the dense, voids-free films with enhanced resis-

tance to cracking in the zone T of the SZM can be formed without

the substrate heating by increasing of the energyE p at low sputter-

ing gas pressures p. The energy E p can be delivered in the growing

filmeither bythe combinedactionof bombarding ions andfastneu-

trals (E p = Ebi + Efn) or bythe fast neutrals only (E p = Efn). The energy

of bombarding ions Ebi is controlled by the substratebiasU s. Onthe

contrary, the energy of condensing fast neutrals Efn is controlled bythe sputtering gas pressure pAr and is increased by decreasing of

the sputtering gas pressure pAr. The whole kinetic energy of these

particlesis transferred to the growing film andstimulatesits densi-

fication and nano-crystallization. This means that the formation of

the flexible, dense, voids-free sputtered films with enhanced resis-

tance to cracking on unheatedsubstrates basedon the replacement

of the conventional heating (T s) with the atomic scale heating (E p)

is possible [22]. There are two key parameters which decide on

the formation of such films: (1) the energy E p and (2) the melting

temperatureT m of created films. More details can be found in Refs.

[13,14,23–26].

In summary, it can be concludedthatthe films with dense,voids-

free microstructure, compressive macrostress ( < 0)and enhanced

resistance to cracking can be formed in the zone T of the Thorn-ton’s SZM also at low substrate temperaturesT s≤100 ◦C,i.e. atlow

values of T s/T m ratio, when sufficient energy E p is delivered to the

growing film by bombarding ions and/or when a low sputtering

gas pressure p is used. Very important role in the low-temperature

sputtering of the flexible films plays also the melting temperature

T m of the film material which (i) decides on the value of T s/T mratio and(ii) canbe controlled by the addition of selected elements

in the film.

5. Conclusions

The investigation reported in this article shows that the brittle

film can be protected against cracking when it is over-coated with

the elastic topfilm. It was found that (i)the brittle films exhibit low

elastic recoveryW e < 60% and low ratio H /E * ≤0.1 and can be either

X-ray amorphous or crystalline, (ii)the elastic top filmsexhibithigh

elastic recovery W e ≥60% and high ratio H /E * ≥0.1 and also can be

either X-ray amorphous or crystalline, and (iii) the cracking of the

brittle filmcan be preventedwhen it is over-coated with the elastic

top film. Thelast finding is of keyimportance notonly for the deep-

ening of the present knowledge in the field of two-layer coatings

but also for many applications. Many functional coatings are brittle

and easily crack when they are (i) deposited on the flexible sub-strates or (ii) bended and thus their function can be interrupted.

Therefore, the overlapping of the brittle film by the elastic top film

(over-layer) is a very efficient tool which ensures the reliable func-

tion of the brittle film even in the case when it is deposited on

the flexible substrate. These conclusions are applicable also to the

films on plastic substrates and the thick multilayer coatings with

alternating brittle/elastic bi-layers.

Acknowledgement

This work was supported by the project LO1506 of the Czech

Ministry of Education, Youth and Sports.

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