Chin. Phys. B Vol. 25, No.

1 (2016) 018101

Effect of fluence and ambient environment on the surface and

structural modification of femtosecond laser irradiated Ti∗
Umm-i-Kalsoom1,2† , Shazia Bashir2 Nisar Ali1,2,3 , M. Shahid Rafique4 ,
Wolfgang Husinsky1 , Chandra S. R. Nathala1 , Sergey V. Makarov5 , and Narjis Begum6
1 Institute for Applied Physics, Vienna University of Technology, Vienna, Austria
2 Centre for Advanced Studies in Physics, GC University Lahore, Pakistan
3 Department of Basic Sciences and Humanities,University of Engineering and Technology Fasalabad, Pakistan
4 Department of Physics, University of Engineering and Technology Lahore, Pakistan
5 P. N. Lebedev Physics Institute RAS, Moscow, Russia
6 Department of Physics, COMSATS Institute of Information and Technology, Islamabad, Pakistan

(Received 16 May 2015; revised manuscript received 27 August 2015; published online 0 X 2015)

Under certain conditions, ultrafast pulsed laser interaction with matter leads to the formation of self-organized conical
as well as periodic surface structures (commonly reffered to as, laser induced periodic surface structures, LIPSS). The
purpose of the present investigations is to explore the effect of fsec laser fluence and ambient environments (Vacuum &
O2 ) on the formation of LIPSS and conical structures on the Ti surface. The surface morphology was investigated by
scanning electron microscope (SEM). The ablation threshold with single and multiple (N = 100) shots and the existence
of an incubation effect was demonstrated by SEM investigations for both the vacuum and the O2 environment. The phase
analysis and chemical composition of the exposed targets were performed by x-ray diffraction (XRD) and energy dispersive
x-ray spectroscopy (EDS), respectively. SEM investigations reveal the formation of LIPSS (nano & micro). FFT d-spacing
calculations illustrate the dependence of periodicity on the fluence and ambient environment. The periodicity of nano-scale
LIPSS is higher in the case of irradiation under vacuum conditions as compared to O2 . Furthermore, the O2 environment
reduces the ablation threshold. XRD data reveal that for the O2 environment, new phases (oxides of Ti) are formed. EDS
analysis exhibits that after irradiation under vacuum conditions, the percentage of impurity element (Al) is reduced. The
irradiation in the O2 environment results in 15% atomic diffusion of oxygen.

Keywords: LIPSS, ablation threshold, incubation coefficient, structural modification

PACS: 06.60.Ei, 06.60.Jn, 07.78.+S, 07.85.Jy DOI: 10.1088/1674-1056/25/1/018101

1. Introduction that it has a vast variety of applications in various fields, like

fuel cells, biomedical engineering, material science, etc. [3,5–7]
Femtosecond (fsec) laser radiation can under certain con-
In this paper we report the dependence of the growth of
ditions induce “periodic surface structures” or LIPSS on the
conical structures and LIPSS on laser fluence and the ambi-
surfaces of metals, semiconductors, and dielectrics. The most
ent environment (Vacuum & O2) . The surface properties of
important parameter which determines the development of
the laser-irradiated Ti samples have been analyzed by using
these structures is the laser fluence. The formation of ripples
SEM, whereas structural modification such as phase analysis
have been observed only in specific fluence regimes (relatively
and chemical composition were explored by XRD and EDS.
low and moderate laser fluence). Furthermore, a possibility for
controlling the periodicity of LIPSS can be achieved by adjust-
ing laser fluence, the number of pulses, pulse width, etc. In 2. Experimental setup
particular, the environmental conditions under which the tar- A chirped pulse amplification (CPA) Ti: Sapphire laser
get is exposed. [1,2] Oliveira et al. [3] studied the formation of amplifier seeded from a mode-locked Ti: Sapphire oscillator
LIPSS and microcolumns on the surface of Ti for various fsec (FEMTOPOWER PRO) was used for the ablation of Ti tar-
laser fluences (0.5–2 J/cm2 ) in stationary and scanning modes. gets. The system was operating at a central wavelength of
They concluded that ripples convert into microcolumns as they about 800 nm, a repetition rate of 1 kHz, with a pulse dura-
are subjected to fluences near the melting threshold of Ti. The tion of about 30 fsec. The beam was focused through a lens of
formation of a regular array of sharp nano/micro conical struc- focal length 20 cm.
tures on Ti using fsec lasers in non-reactive (vacuum and He) Rectangular-shaped Ti targets with a dimension of
as well as in reactive medium (SF6 , air or HCl) has also been 20 mm×15 mm×3 mm were ground, polished (upto a rough-
reported. [4] The importance to explore the structuring of Ti is ness value of 1 µm), and ultrasonically cleaned with acetone
∗ Project
supported by Österreichische Forschungsfödergesellschaft (FFG) (Grant No. 834325).
† Corresponding
author. E-mail: [email protected]
© 2016 Chinese Physical Society and IOP Publishing Ltd 　http://cpb.iphy.ac.cn
http://iopscience.iop.org/cpb　

018101-1
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101
for 30 minutes before irradiation. These targets were mounted The XRD technique was employed for phase analysis by using
on a target holder placed in a vacuum chamber that was evac- an X’Pert PRO (MPD) x-ray diffractometer. The EDS analysis
uated to a base pressure of the order of 10−3 mbar. Two sets was performed for chemical analysis of irradiated targets.
of experiments were performed. (i) Exposure of Ti targets by
a single laser pulse for various energies (20, 30, 40, 50, 60, 70, 3. Results and discussion
80, 130, 180, and 230 µJ) corresponding to fluences of 0.38,
3.1. Morphological results using SEM analysis
0.57, 0.86, 1.00, 1.13, 1.27, 1.52, 2.47, 3.42, and 4.37 J·cm−2 ,
respectively . SEM micrographs in figure 1 show the modified surface
The results obtained from this set of experiments were of Ti for various laser fluences of (a) 0.86, (b) 1.00, (c) 1.13,
mainly utilized to determine the single shot ablation thresh- (d) 1.27, (e) 1.52, (f) 2.47, (g) 3.42, and (h) 4.37 J·cm−2 . (i)
old fluence and estimate the incubation coefficient of Ti. The Full view for the fluence value of 4.37 J·cm−2 after irradiation
ablation threshold was evaluated by plotting the squared spot with 100 laser shots under vacuum conditions. Various fea-
diameter (D2 ) (obtained by SEM micrographs) versus the log- tures, like, craters, cones, and LIPSS (ripples) are observed on
arithm of the laser pulse energy. From the slope of this graph the surface of irradiated Ti. Ripples formed on the irradiated
the value of spot size is calculated to be 58 µm and the Ti surface are of two kinds, i.e., micro and nano scale. It has
threshold energy was determined by extrapolating the graph been demonstrated in Refs. [8] and [9], that nano-scale (sub-
to zero. (2) Exposure of Ti targets to 100 laser pulses for var- wavelength) ripples are oriented perpendicular to the direction
ious fluences of 0.86, 1.00, 1.13, 1.27, 1.52, 2.47, 3.42, and of linear polarization of laser beam. Whereas the micro-ripples
4.37 J·cm−2 . Results obtained in the second set of experiments are oriented in the direction parallel to the linear polarization
have been presented. Both sets of experiments were performed of the incident laser beam. Nano-scale ripples are observed
under a vacuum as well as in the O2 environment at a pressure for all maximal laser fluences but in different areas of the
of 133 mbar. laser spot. For lower maximal fluences (0.86 to 1.13 J·cm−2 ),
Surface morphology of the irradiated Ti targets was in- formation of nano-scale ripples is observed closer to the cen-
vestigated by using SEM (FEI-QUANTA 200F, Netherlands). ter. However, at high maximal fluences, ranging from 1.27

(a) (b) nano (c) nano

nano
ripples ripples ripples

(d) (e) (f)

cavities cavities cones

cones nano nano cavities
nano
ripples micro ripples ripples
ripples cones
micro
ripples

(g) (h) (i)

cavities cavities

cones cones
nano
ripples

Fig. 1. SEM images revealing the variation in the surface morphology of Ti after ablation by 100 pulses of fsec laser at wavelength of 800 nm,
pulse duration of 30 fsec, and repetition rate of 1 kHz for various fluencies of (a) 0.86, (b) 1.0, (c) 1.13, (d) 1.27, (e) 1.52, (f) 2.47, (g) 3.42, (h)
4.37 J·cm−2 and (i) full view of the ablated region for a fluence value of 4.37 J·cm−2 under vacuum (10−3 mbar) conditions.

018101-2
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101
to 4.37 J·cm−2 , nanoripples are formed only in the periph- free electron density due to this surface roughness plays a
eral ablated areas. While at the center features including mi- significant role in the development of nano-scale ripples. [16]
croscale ripples, conical structures and cavities are observed The formation of nanoripples has also been explained on the
as seen in Figs. 1(d)–1(h). The average spacing of micorip- basis of a parametric decay (stimulated Raman scattering)
ples is about 2 µm, which is significantly greater than the inci- model. [10] In this model, the plasma wave travels slowly, at
dent laser wavelength (Fig. 1(d)). In the highest fluence areas a speed of less than 10−2 times the speed of light and an ion-
(2.47–4.37 J·cm−2 ) (Figs. 1(f)–1(h)), micro-scale ripples also enriched local area appears. Before the next peak of an elec-
vanish completely and only microconical structures and cav- tron wave arrives, ions experience a strong coulomb repulsive
ities remain visible. This implies that for both nano as well force causing a coulomb explosion. Through this process, pe-
as microscale ripples, there is a certain fluence window below riodic ripple structures may be formed. [10]
which they are not formed, above which they are destroyed.
However, the threshold fluence for the formation of nanorip-
ples is smaller than that for microripples. This information is (a)

compatible with previously reported work by many research

groups. [9,10]
nano
For precise measurement of nanoripples formed on the ripples
Ti surface, fast Fourier transform (FFT) was employed for all
fluences. The enlarged SEM view of nano-ripple formation of
Fig. 1(a) is shown in Fig. 2(a). Figure 2(b) corresponds to the
2D FFT image for Figs. 1(a) and 2(c) reveals the variation in
5 mm
periodicity of nano-LIPSS for various laser fluences.
In order to reveal the variation in the LIPSS periodicity
versus local fluence, the following equation was used to eval- (b)

uate local fluence: [11]

1 DLIPSS0 2
   
ϕmin = ϕ0 exp − , (1)
2 ω0

where ϕmin is the local fluence for which nano-LIPPSS ap-

pears, ϕ0 is the peak fluence, DLIPSS0 (128 to 91 µm) is the
inner diameter of the surface region in which nano LIPSS are
formed and ω0 is the beam waist radius (58 µm). The values of
local fluence vary from 0.08 to 1.28 J·cm−2 with the increase
of peak fluence from 0.86 to 4.37 J·cm−2 . The periodicity of (c)
nano ripples reduces from 700 to 490 nm with the increase 700
of local fluence from 0.08 to 1.28 J·cm−2 (for peak fluencies
Periodicity/nm

from 0.86 to 4.78 J·cm−2 ) as shown in Fig. 2(c).

600
The reduction in periodicity, for various semiconducting
materials have been studied by different research groups. [12,13]
500
This decrease in the periodicity has been explained on the ba-
sis of coupling between surface plasmons and incoming laser
radiation. [13] As the surface gratings formed during the first 400
0 0.4 0.8 1.2
few pulses, the resonant wavelength of surface plasmons un- Local fluence/JScm-2
dergo blueshift. This shift causes the reduction of periodicity Fig. 2. (a) Magnified view of nano-LIPSS formation of Figs. 1(a)
with the increase of fluence or the number of pulses. The re- and 1(b). Two-dimensional fast Fourier transform (FFT) spectra of
Figs. 1(a) and 1(c). The variation in periodicity of nano-LIPSS for
duction in the periodicity can also be attributed to the increas- various local fluences using FFT after ablation of Ti under vacuum
ing refractive index of Ti after enhancement of surface rough- (10−3 mbar) condition by 100 pulses of fsec laser at wavelength of
800 nm, pulse duration of 30 fsec, and repetition rate of 1 kHz.
ness due to laser irradiation that significantly affects the prop-
agation of surface plasmons. [14] The generation of nanoripples On the other hand, microripples are formed through rapid
has been explained on the basis of surface plasmons (SP’s) or a heating and melting of the surface layer followed by fast cool-
parametric instability. [15] During laser irradiation, the first few ing under plasma pressure and gradients in the thermodynamic
pulses create and enhance the surface roughness. Non-uniform parameters. [17]
018101-3
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101
Laser-induced cavities can serve to compress the laser- 4.37 J·cm−2 after irradiation with 100 laser shots in O2 envi-
induced plasma and therefore can initiate an extreme non- ronment at a pressure of 133 mbar. The formation of both nano
equilibrium state followed by self organization that results in and micro (1 µm) LIPSS is observed. They are similar in ap-
the formation of micro ripples. [18] The formation of cavities pearance to the ripples that have been observed under vacuum
under compressed plasma flow can be related to the violent conditions (Fig. 1).
boiling and bubble formation in the superheated liquid layer. Comparison of the two ambient environments, vacuum
Due to the turbulence and thrust of the boiling bubbles inside and O2 (Figs. 1 and 3), shows that the fluence threshold for
the liquid layer followed by a rapid cooling leads to the for- microstructure formation is lower in the case of oxygen, as
mation of cavities and frozen melt in the form of microconical compared to a vacuum environment. The presence of the gas
structures. [19] helps to accelerate the formation of these surface structures,
SEM images of Fig. 3 show the modified surface of Ti for due to confinement effects [20] and enhancement in the thermal
various laser fluencies. (i) Full view for the fluence value of energy coupling. [21]

(a) (b) (c)

nano nano
ripples ripples
cavities
cones
nano
micro ripples
ripples
10 mm 10 mm 10 mm

(d) (e) (f)

cavities
micro
ripples cavities
cones cavities
nano nano
nano cones ripples cones
ripples ripples

10 mm 10 mm 10 mm
nano
(g) (h) (i) ripples

10 mm
cavities cones
cavities

cones
10 mm 10 mm 100 mm

Fig. 3. SEM images revealing the variation in the surface morphology of Ti after ablation by 100 pulses of fsec laser at a wavelength of 800 nm,
pulse duration of 30 fsec, and a repetition rate of 1 kHz for different fluences of (a) 0.86, (b) 1.0, (c) 1.13, (d) 1.27, (e) 1.52, (f) 2.47, (g) 3.42,
and (h) 4.37 J·cm−2 . (i) Full view of ablated region for a fluence value of 4.37 J·cm−2 in O2 at a pressure of 133 mbar.

Fast Fourier transform (FFT) has been employed for all from 640 to 410 nm. This shows that comparatively fine rip-
fluences in order to measure the variation in periodicity of ples with slightly less periodicity are formed in the O2 envi-
nano ripples on irradiated Ti surface in O2 ambient. The en- ronment as compared to the vacuum condition. A possible
larged SEM view of nano-ripple formation of Fig. 3(a) shown explanation for this fact are confinement effects of O2 (at a
in Figs. 4(a) and 4(b) corresponds to a 2D-FFT image because pressure of 133 mbar), which prevents the free expansion of
figures 3(a) and 4(c) show the variation in periodicity of nano-
the plume and random movement of ejected material during
LIPSS for various local fluences. The value of periodicity of
laser ablation and serves for the fixation of surface waves, in
ripples reduces monotonically from 640 nm to 410 nm, with
a well defined manner. [20] This confinement can induce more
the increase of local fluence from 0.01 to 0.6 J·cm−2 .
It is found that the environments (vacuum & O2 ) play a energy and pressure [22] as compared to a vacuum and conse-
significant role for the growth and periodicity of LIPSS. In the quently, fine nanoripples with smaller periodicity are grown,
case of a vacuum, the periodicity of ripples varies from 700 which is also compatible with the results presented in Figs. 2
to 490 nm, whereas in the case of O2 , the periodicity varies and 4.
018101-4
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101

(a) 700
(b)
(c)

Periodicity/nm
600
nano
ripples

500

5 mm 400
0 0.2 0.4 0.6
Local fluence/JScm-2
Fig. 4. (a) Magnified view of nano-LIPSS formation of Fig. 3(a). (b) two-dimensional fast Fourier transform (FFT) spectra of Fig. 3(a), and (c)
Variation in periodicity of nano-LIPSS for various local fluences using FFT after ablation of Ti in O2 by 100 pulses of fsec laser at wavelength
of 800 nm, pulse duration of 30 fsec and repetition rate of 1 kHz

3.2. Quantitative analysis the ablation threshold and the incubation factor, the Ti targets
were exposed to single and 100 laser shots. The irradiation
3.2.1. Ablation threshold and incubation factor
was performed under a vacuum and O2 environment for differ-
The ablation threshold fluence and incubation factor are ent pulse energies. The threshold fluence and the incubation
important considerations to understand the origin of ablation, factors were then derived from the SEM images of the exposed
when a laser interacts with a material. In order to determine targets.

40000 40000
(a) (b)
32000 32000
D2/mm2

D2/mm2

24000 24000

16000 16000

8000 8000

2 3 4 5 6 2 3 4 5 6
ln(E)/mJ ln(E)/mJ

40000 48000
(c) (d)
40000
32000
32000
D2/mm2

D2/mm2

24000
24000
16000
16000

8000 8000
2 3 4 5 6 2 3 4 5 6
ln(E)/mJ ln(E)/mJ

Fig. 5. Plot of squared spot diameter (D2 ) versus the logarithm of the laser pulse energy under a vacuum (10−3 mbar) for (a) single pulse, (b)
100 pulses, and in O2 environment at 133 mbar pressure for (c) single pulse and (d) for100 laser pulses.

Figures 5(a)–5(d) show the variation in the squared spot spot size (ωf ) was determined from the slope of the linear fit
diameter (D2 ) as a function of log (ln) of the pulse energy for (Fig. 5). The threshold energy (Eth ) was determined by ex-
single (a, c) and 100 pulses (b, d) in both environments. The
spot diameter was measured by using SEM images for sin- trapolating the D2 to zero. The ablation threshold fluence was
gle and multiple (100) pulse experiments. The focused beam calculated by using the following equation: [23]
018101-5
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101
2Eth slight decrease in the peak intensity of the (100) plane is ob-
ϕth = . (2)
πωf2 served, which may be due to structural defects caused by irra-
The calculated values of the ablation threshold for single and diation.
multiple (100) shots are listed in Table 1. It is clear that the 20000 Ti
ablation threshold in an O2 environment is lower than in a vac-

Intensity/arb. units
uum. This is associated with an enhancement of the thermal 15000
energy coupling during laser ablation, which is more domi- 4.37 JScm-2

nant in a gaseous medium than in a vacuum. [21] The other 10000 2.47 JScm-2

possible important factor responsible for the smaller value of 1.13 JScm-2
the ablation threshold in O2 is the confinement effect that 5000 0.86 JScm-2
enhances collisions between the ablated species and the gas
untreated
molecules. [24] In a reactive gas, the high temperature and pres- 0
sure in the plume result in the formation of gas molecule rad- 20 40 60 80
icals. The reactions between ablated products and these gas 2θ/(Ο)
Fig. 6. (color online) X-ray diffractograms of pristine and laser-
radicals promote condensation and induce a faster structure
irradiated Ti exposed to various fluences of 0.86, 1.13, 2.47, and
growth, which in turn reduces the ablation threshold. [24] 4.37 J·cm−2 under vacuum (10−3 mbar) conditions.

Table 1. Calculated values of ablation threshold fluence and incubation Figure 7 shows the x-ray spectra of the pristine and ir-
coefficient of Ti, for single and multiple (100) pulses, for both ambient
conditions (vacuum and O2 ) after ablation by fsec laser at a wavelength radiated Ti exposed for the same conditions but in an O2 en-
of 800 nm, pulse duration of 30 fsec and repetition rate of 1 kHz. vironment. For the low irradiation fluencies, no new phases
Threshold fluence Under vacuum condition In O2 (133 mbar) are observed. However, for the highest maximal fluence, i.e.,
ϕth (1)/J·cm−2 0.13 0.093
4.37 J·cm−2 , several new phases of oxides TiO2 (110), Ti3 O
ϕth (100)/J·cm−2 0.09 0.048
incubation Co-efficient 0.83 0.85
(201), TiO2 (220), TiO2 (311), TiO2 (320) are identified. For
maximal fluence, melting of the target is maximal and ioniza-
With increasing the number of laser shots from single to tion of the ambient gas is very high, which increases the reac-
100 for both environments, a reduction in the ablation thresh- tion rate between the molten layers of Ti and atomic oxygen.
old is observed. This reduction of the threshold can be at- This reaction during the resolidification causes the formation
tributed to an incubation effect. [25] In case of metals, the in- of several new phases of oxides of Ti. The diffusion of reac-
cubation behavior is due to the accumulation of plastic defor- tive gas atoms to interstitial sites can be clearly observed for
mation caused by laser-induced thermal stresses. [26] The incu- this fluence. [29] The presence of O2 is also confirmed by EDS
bation coefficient has been evaluated by using the following analysis (Table 2).
power law: [27]
Ti3O TiO2 Ti
Φth (N) = Φth (1)N S−1 , (3) 6000
Intensity/arb. units

where Φth (N) is the threshold fluence for N laser shots (100 in
4000 4.37 JScm-2
our case), Φth (1) is the single-shot ablation threshold fluence,
and S is the incubation coefficient. Calculated values of the 2.47 JScm-2
2000
incubation coefficients are also listed in Table 1. 1.13 JScm-2

0.86 JScm-2
3.3. XRD analysis 0 untreated
In order to explore the structural changes in the ablated 20 40 60 80
Ti, an XRD analysis was performed. Figure 6 shows the 2θ/(Ο)

x-ray diffractograms of pristine and laser-irradiated Ti ex- Fig. 7. (color online) X-ray diffractograms of pristine and laser-
irradiated Ti exposed to various fluences of 0.86, 1.13, 2.47, and
posed to various maximal laser fluences (0.86, 1.13, 2.47, and 4.37 J·cm−2 in ambient environment of O2 at 133 mbar pressure.
4.37 J·cm−2 ) under vacuum conditions. In case of pristine Ti,
hexagonal phases of Ti (100), (002), (101), (102), (110), (103), 3.4. EDS analysis
(112), and (201) (Pattern No. 01-089-2959) are identified. A chemical analysis of the pristine and fsec laser irradi-
The XRD patterns of the irradiated Ti do not show formation ated Ti targets at a maximal laser fluence of 4.37 J·cm−2 under
of new phases, which indicates that residual thermal stresses vacuum conditions and in the presence of O2 at 133 mbar pres-
were not high enough to create new reflection planes. [28] A sure is shown in Table 2. A percentage error of about ±5% can
018101-6
 Chin. Phys. B Vol. 25, No. 1 (2016) 018101
be assumed for all tabular data. The untreated target of Ti con- and third authors for a six months visit to Technical University
sists of 94% Ti and 6% Al. After irradiation under vacuum Vienna, Austria under the “International Research Support Ini-
conditions, the Al content reduces to 2% with the increased Ti tiative Program (IRSIP)”.
content up to 98%. Whereas, during irradiation in an O2 envi-
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The first and third authors are thankful to the Higher Ed- [30] Biao Y, Wang G, Yong Y, Wang Z and Peng X 2015 Acta Phys. Sin. 6
ucation Commission (HEC) of Pakistan, for funding the first 026602 (in Chinese)

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