Micro-Raman mapping of micro-gratings in BACCARAT glass directly written

using femtosecond laser

K.C. Vishnubhatla,
1,4,6
S. Venugopal Rao
2,*
, R. Sai Santosh Kumar,
1
S.N.B. Bhaktha
3
,A. Chiappini,
4
A.
Chiasera,
4
J. Laureyns,
3
M. Ferrari,
5
M. Mattarelli,
4
M. Montagna,
4
R.Osellame
6
, R. Ramponi
6
, G.C.
Righini
7
, S. Turrell,
3
and D. Narayana Rao
1,#

1
School of Physics, University of Hyderabad, Hyderabad 500046, India
2
Advanced Centre of Research in High Energy Materials (ACRHEM), School of Physics
University of Hyderabad, Hyderabad 500046, India.
3
Universit des Sciences et Technologies de Lille, Laboratoire de Spectrochimie Infrarouge et Raman, LASIR UMR
8516 du CNRS - Bt C5, 59655 - Villeneuve d'Ascq cedex, France
4
Dipartimento di Fisica, CSMFO Group, Universit di Trento, Via Sommarive 14, 38050 Trento, Italy
5
IFN-CNR, Istituto di Fotonica e Nanotecnologie, CSMFO Group, Via Sommarive 14,
38050 Trento, Italy
6
Istituto di Fotonica e Nanotecnologie, Consiglio Nazionale delle Ricerche, Istituto Nazionale per la Fisica della
Materia, Dipartimento di Fisica, Politecnico, Piazza L. da Vinci, 32, I-20133 Milano, Italy
7
Department of Optoelectronics and Photonics, Nello Carrara Institute of Applied Physics, IFAC-CNR,
Via Panciatichi 64, I-50127 Firenze, Italy
ABSTRACT
We present some of our results on the femtosecond laser direct writing and characterization of micro-gratings in
Baccarat glass. Gratings were inscribed with amplified 800 nm, ~100 femtosecond pulses at 1 kHz repetition rate. The
change in refractive index of the modified region was estimated from grating efficiency measurements and was found to
be ~10
-3
. Micro-Raman studies demonstrated an increase in the intensity of the band near 596 cm
-1
in the laser irradiated
region clearly indicating an increase in the refractive index. Micro-Raman mapping of the grating showed a periodic
variation of the band intensity further confirming the formation of grating. Structures with sub wavelength dimensions
(<800 nm) were achieved with shaping of the input pulses using a rectangular slit. Waveguides were inscribed by
optimizing parameters like slit width, focusing conditions, translation speed etc. We shall present our results on the
physical, spectroscopic and optical characterization of these structures.
Keywords: Laser Direct Writing, Micro-Raman, gratings
1. INTRODUCTION
Recent advances in femtosecond laser direct writing (LDW) demonstrate unprecedented prospects for
miniaturization and integration of highly functional photonic and microfluidic devices directly inside transparent
dielectric and polymeric materials.
1-12
Femtosecond pulses possess the unique ability to precisely deposit energy inside
the material and significantly the ultrafast interaction does not require specially prepared or photosensitive materials
unlike other fabrication techniques. This technique is attractive for fabrication of photonic structures in rare-earth
activated glasses for creating gain elements and waveguide lasers
13
and structures for microfluidics.
14,15
We have
recently established the efficacy of Er activated Baccarat glass as a potential candidate for applications in
telecommunications with good spectroscopic properties and high quantum efficiency, close to 80%.
16
Here, we present
some of our results on the direct writing and characterization of micro-gratings and waveguides in Baccarat glass.
Gratings were inscribed with amplified 800 nm, ~100 femtosecond pulses at 1 kHz repetition rate. Structures with sub
wavelength dimensions (< 800 nm) were achieved with shaping of the input pulses using a rectangular slit. Waveguides
were inscribed by optimizing parameters like slit width, focussing conditions, translation speed etc. The change in
refractive index of the modified region was estimated to be ~10
-3
from grating efficiency measurements. The modified
structures were studied by micro-Raman spectroscopic technique.
________________________________________________________________
e-mail:
*
[email protected], # [email protected], Fax: +91-40-23011230
Commercial and Biomedical Applications of Ultrafast Lasers VIII, edited by Joseph Neev,
Stefan Nolte, Alexander Heisterkamp, Christopher B. Schaffer, Proc. of SPIE Vol. 6881, 688114,
(2008) 0277-786X/08/$18 doi: 10.1117/12.762707
Proc. of SPIE Vol. 6881 688114-1
M a i t a i N '
" M 1 , M 2 , M 3 M i r r o r s
( o s c i l l a t o r )
R S R e c t a n g u l a r S l i t
R S
( w i t h M i c r o m e t e r )

M O - M i c r o s c o p e O b j e c t i v e
_ _ _ _ _ _ _ _
N D - N e u t r a l D e n s i t y f i l t e r
S p i t f i r e
S a m p l e
X Y Z - N a n o s t a g e


2. EXPERIMENTAL
The glass has been produced at Cristallerie Baccarat by a conventional melt-quenching technique with the
following molar composition: 77.29 SiO
2
: 11.86 K
2
O: 10.37 PbO: 0.48 Sb
2
O
3
. The density of the samples has been
measured by a gas pycnometer. The Er
3+
concentrations have been determined to be 0.2 mol%, taking into account both
the nominal composition and the measured density of the glass. Refractive index value at several wavelengths has been
measured to be 1.5427 with an accuracy of 0.001 and resolution of 0.0005, using a standard prism coupling method.
17

2.1 Spectroscopic characterisation of glass:
Optical absorption experiments were performed at room temperature from the ultraviolet to the near infrared
spectral range with a double beam spectrophotometer (UV-Vis-NIR Cary 5000 Varian). The Fourier Transform Infrared
(FTIR) spectroscopy measurements were carried out by using a JASCO FTIR-660 plus spectrometer with a resolution
set to 4 cm
-1
. The polarized VV and depolarized HV Raman spectra were obtained by exciting the samples with the 488
nm line of an Ar
+
-ion laser. The signal was selected by a double monochromator and analyzed by a photon-counting
system. The 514.5 nm line of an Ar
+
-ion laser and the 980 nm line of a Ti:Sapphire laser were used as excitation sources
for near infrared photoluminescence (PL) spectroscopy measurements. A Triax 320-mm-focal-length single-grating
monochromator was used to disperse the luminescence light onto an InGaAs photodiode and the signal acquisition was
performed using a standard lock-in technique. To measure the PL decay of the excited
4
I
13/2
level, the continuous wave
excitation laser was pulsed with a mechanical chopper and data were acquired with a digital oscilloscope.
2.2 LDW experimental set up :












Figure 1 Schematic diagram of laser Direct writing setup
The sample was typically cut to a dimension of 1 cm X 2 cm X 0.5 cm (thickness)) for ease of use and all the 6
faces were optically polished. The sample was first cleaned using acetone and then with methanol to ensure the surface
is devoid of any stains and dust. The cleaned sample was placed on computer controlled XYZ nanostages for better
control over the structures to be written in them. Figure 1 shows the schematic of the experimental setup used for direct
writing. The quality of the structures fabricated depended critically on the quality of the focused spot and the movement
of the sample placed on XYZ stage. Any aberration in the optics or stage movement will affect the shape and size of the
structures drastically. Typically 100 fsec pulses from a femtosecond amplifier were employed for direct writing at a
wavelength of 800 nm with 1 KHz repetition rate. Neutral density filters were used to attenuate the energy of the input
beam. The beam was steered such that it focuses downwards on to the sample after the microscope objective (typically
40X with 0.65 NA). A rectangular slit whose width could be varied from 500 m to 2 mm was used to modify the
spatial profile of the input beam for improved structures.
Proc. of SPIE Vol. 6881 688114-2


2.3 Inscription of grating:

The procedure followed for inscribing and characterizing the gratings is as follows. Initially simple straight line
structures were inscribed into samples. Each line corresponded to a specific set of parameters (like the sample
translation speed, input energy of the fsec pulses, and size of the aperture before the microscope objective). Later these
structures were imaged using Leica scanning confocal microscope. Images were obtained both in transmission mode
and reflection mode. The imaging essentially takes advantage of deferential transmission and reflection properties of the
samples in the regions exposed to the femtosecond laser and the un-exposed regions. In the transmission mode the width
of the structures was determined. In the reflection mode several snapshots of the structures were taken along the depth at
definite intervals (typically the step size along the z is chosen to be ~1 m). Each snapshot corresponded to a particular
depth and all these snapshots were collated to obtain a 3-D (cross-sectional, depth profile) view of the structures written.
In the transmission mode the width of the structures is determined. The lines/structure with desired width and depth
profile were identified and with the corresponding writing parameters the structures/lines were written again and the
images compared to ensure the reproducibility.
3. RESULTS AND DISCUSSION

Raman and absorption measurements indicate the high transparency of the Baccarat glass. The water content of
these glasses is very low and we estimate a C
OH
concentration as low as 3.6x10
18
cm
-3
. Luminescence at 1.5 m with a
spectral width of ~18 nm was observed on both the glasses. No changes in the spectral width as a function of the
excitation wavelength were observed and no NIR-to-visible up-conversion signal has been detected. The non-appearance
of up-conversion in Baccarat glasses indicates that most of Er
3+
ions are homogeneously distributed and that
interaction clusters as well as chemical clusters are practically absent. The
4
I
13/2
metastable state of the Er
3+
ions decay
curve present a single exponential profile, with a lifetime value of 14.2 ms for the sample doped with 0.2 mol % of
erbium. Radiative lifetime were calculated with different models and compared with the experimental measured
lifetimes. For the 0.2 mol % Er
3+
-activated glass, quantum efficiency reaches very high values, up to 79.8 % in the case
of a calculation based on the Judd-Ofelt theory. Such high quantum efficiency has already been observed in Er
3+
-doped
tellurite glasses and remains among the highest quantum efficiencies estimated in pure or modified-silica host glasses.
The optical and spectroscopic properties of this modified-silica glass make it well adapted as host medium for the light
propagation and a good candidate for many applications in telecommunication systems.
16
3.1 Efficiency measurements and Micro-Raman mapping of the gratings
Figure 2 (a) shows the confocal microscopic image of the grating structure inscribed in the glass. A continuous
wave He-Ne laser was diffracted through the grating and the internal diffraction pattern was captured on a screen (see
figure inset). The intensity of the diffraction orders (0, 1) were obtained and the diffraction efficiency was calculated to
be ~17%. From the diffraction efficiency measurements the estimated change in the refractive index was ~2.2 10
-3

using the relation n = cos() tanh
-1
( )/d, where is the diffraction efficiency fraction of first order to the zeroth
order; d is the depth or the grating thickness; = 90 degrees; is the wavelength. The periodicity of the gratings was 6
m. The periodicity and the grating width could be controlled through the input energy, scan speed, and the focal
conditions. We could achieve grating periods (and spacing) ranging from 4 m to 10 m easily. The modified region
was studied by micro-Raman spectroscopy for an insight into the physical changes which occurred at the focus due to
fsec pulses interaction. Two main differences between irradiated and not irradiated lines were observed 1) an increase of
the sharp defect band at 596 cm
-1
and 2) an increase of intensity and line width of the broad band at about 470 cm
-1
. This
corresponds to a hardening of the structure by irradiation, which can be associated to a positive change of the refractive
index.
The micro-Raman mapping of the grating structure was done across three lines of the grating. The rectangular
area highlighted in the figure 3 (a) was the region of the sample mapped and 3(b) shows the results of the mapping of
Raman intensity. The periodic variation of Raman intensity further proved the grating structure formation and also
reflects the periodic refractive index variation across the grating structure.
Proc. of SPIE Vol. 6881 688114-3
( a )
U
( b )














Figure 2 (a) Microscope image of the grating inscribed into baccarat glass; the inset shows the internal diffraction pattern. (b)
The Raman spectrum from the laser modified region (red, dashed curve) and unmodified region (black, solid curve).














Figure 3 (a) Optical image of the grating inscribed into baccarat glass; the rectangular highlighted region was mapped for intensity (b)
Raman intensity map of the rectangular region in (a) with bright region of the map indicating higher intensity
4. SLIT BEAM SHAPING FOR LDW TO FABRICATE MICRO STRUCTURES
AND WAVEGUIDES

There are two principle ways of LDW a) Transverse configuration, where the sample translation is perpendicular
to laser propagation and b) Longitudinal configuration, where the sample translation and the laser beam propagation are
200 400 600 800 1000 1200
0.0
0.2
0.4
0.6
0.8
1.0
1.2


R
a
m
a
n

I
n
t
e
n
s
i
t
y

(
a
.
u
.
)
Raman shift (cm
-1
)
Non-irradiated
fsed Irradiated
Proc. of SPIE Vol. 6881 688114-4
I n t e n s i t y ( a v g e n . r g y ) : S O
' h r i e i i y ( v E 4 v r l t g y ) S O p J
S l I t ( w i d t h ) : N o s l . z
S l i t i w . c j N l N o S C i L
L a b e l ; 6 5 6 4 6 2 E r
S p s e d ; & i D 2 5 0 O C 5 0 2 5
L a t e l 0 0 6 7 6 6
S p e e d : S m 2 5 0 l E N ]
n t o n I ' ( A V e n . r y ) I n t . n u i t y ( a v g n . r g y ) : P
i i C i d t h ) N : ; S l i t
1
L a b e l ; J
S p e e d : I Z O 5 0 2 5 1 0 S p e e d
5 2
I C
: i w : ; s i o n S f i t v i d t : i ) N O S l i t


parallel. Longitudinal LDW creates cylindrical waveguides but the length of the waveguides is limited by the working
distance of the focussing objectives.
The transverse writing geometry allows one to write waveguides and structures of arbitrary length and design.
However, this method produces waveguides and structures with strong core asymmetry and significant losses
(particularly in the case of waveguides).
18
This asymmetry can be explained as follows: perpendicularly to the beam
propagation direction the waveguide size is given approximately by the beam focal diameter 2
0
, while along the
propagation direction, it is given by the confocal parameter b = 2
0
2
/.
19
For focused diameters of the order of a few
micrometers this results in a large difference in waveguide sizes in the two directions. This asymmetry becomes
particularly severe when the waveguide size is increased, as required for wave guiding at the optical communication
wavelength of 1.5 m, thus greatly reducing the efficiency of fiber butt coupling in conventional telecommunications
setups.
19


















Figure 4 Confocal microscope images of micro-structures inscribed in Baccarat glass. The parameters of the LDW such as average
energy of the incident laser pulse and the sample translation speeds (m/sec) are given.
To circumvent this problem Osellame et al.
20
introduced a novel focusing geometry in which the femtosecond
writing beam is astigmatically shaped by changing both the spot sizes in the tangential and sagittal planes and the
relative positions of the beam waists. This shaping allowed the modification of the interaction volume in such a way that
the waveguide cross section can be made circular and with arbitrary size.
21
Another simpler way is to use a rectangular
slit oriented parallel to the writing direction.
22
In transverse LDW, by placing a rectangular slit close to the focussing
objective acts as diffractive element and helps in redistribution of the laser intensity gradient around the focus. Various
structures were written by placing a rectangular slit of different dimensions (2 mm, 1.5 mm, 0.5 mm) before the
focussing microscope objective. For a particular slit width line-structures were inscribed by varying the incident laser
intensity and the translation speed of the samples and the process was repeated for all other slit widths mentioned
above. The incident laser energy shown in the figures was measured before the focussing by microscope objective and
after the slit was placed (the typical values of average energy were varied from < 5 J to 75 J). The lower end intensity
was estimated to be in the range 2-5 J taking into account the transmission efficiencies of the slits used and the filters
placed. The higher end was fixed at around 80-90 J, as energies above this were observed to damage samples. The
Proc. of SPIE Vol. 6881 688114-5


typical speeds of the sample translation were 10, 25, 50, 100, 250 and 500 m/second. To avoid sample damage lower
translation speeds (< 50 m /second) were not employed while inscribing micro-structures at higher incident laser
intensities (> 40 J). Similarly higher translation speed were not used at very low incident laser intensities (< 20 J) as
the modifications induced by laser inscription in the samples at such experimental conditions were minimal or
negligible, and they could not be imaged by the confocal microscope even when operated at higher magnifications.























Figure 5 Confocal microscope images of micro-structures inscribed in Baccarat glass. The parameters of the LDW such as average
energy of the incident laser pulse and the sample translation speeds (m/sec) are given. A slit of 0.5 mm was used for beam shaping
The confocal microscope images of the structures written without a slit are shown in figure 4 while the structure
written with a slit of 500 m placed before the focussing objective are shown in the figure 5. We feel that the wobbly
features seen in some of the structures can be avoided by using a vibration isolation optical table for mounting the nano-
positioner. In every figure, it can be seen that the incident femtosecond laser (average) energy and the width of the slit
used are mentioned on the top, while at the bottom the line structure label number and the corresponding speeds (in units
of m/second) at which the sample was translated is mentioned. As seen from the figures the width of the structures
written at lower speed are broader than that written at higher speed. When the sample was moved at lower speeds a
particular region is exposed for more number of laser shots, hence the area modified is more. The structures written
using a slit at moderate laser intensities (20 to 30 J) and at speeds of (250, 500 m/second) appear more smooth on
visual inspection through the microscope as compared to structures written without using slit. For faster speeds of
translation of the sample the structures were smooth irrespective of the usage of slit. The width of the structures could
be varied from 4 m to 10 m with varying speeds and input energy. Some of the structures had interesting features,
Proc. of SPIE Vol. 6881 688114-6
( a ) : 1 ( b ) ! 9 :
L a b e l : S L 4
S p e e d
5 0 0
I n t e n s i t y ( a v g e n e r g y ) 8 0 p J
S l i t
( w i d t h )
: 1 . 5 m m
L a b e l : 1 6
S p e e d
: 1 0 0
I n t e n s i l y ( a v g e n e r g y ) : C
5 J J
S l i t
( w i d t h )
2 m m
L a b e l : 5 1
S p e e d
: 1 0 0
I n t e n s i t y ( a v g e n e r g y ) : C 5 p J
S l i l ( w i d l h ) : 0 . 5 m m


both in perpendicular and parallel direction, with dimensions of the order of <1 m and the reason for the appearance of
these structures is being investigated.
Figure 6 Microscope images of the structures inscribed in the baccarat glass
With the effects due to repetitive exposure of a specific spot and the translation speed some interesting structures
were inscribed in Baccarat glass. Some of the interesting structures produced are depicted in figure 6(a) where the width
of the structure was 750 nm. Such sub-micron structures when created in periodic fashion in three dimensions can lead
to photonics crystals. Selective etching, if possible, of these regions will result in nanochannels. The contiguous pearl
[fig 6 (b)] shaped micro-structure can be used as waveguide attenuators
7
as these structures scatter light. The grating
like structures seen in figure [fig 6 (c)] are parallel to the scale bar, and are periodic with sub-micron dimensions. These
modified planes are perpendicular to the written line structure are similar to the Bragg gratings. With a better control
over dimension and periodicity of the structure, Bragg gratings can be inscribed directly by LDW while simultaneously
inscribing the waveguides. We are investigating the effect of diffraction from the slit used in the variety of structures
produced.

(a) (b)
Figure 7 Typical photographs of the wave guides with He-Ne laser coupled in (a) and no coupling seen in (b)
The optical properties of the structures were tested with the help of a 1560 nm cw laser. The laser light was butt-
coupled into some of these waveguides and near-field mode profiles from the exit end were captured with the help of a
microscope objective and CCD camera. These initial results show that there is indeed a positive refractive index change
sufficient enough for light to be confined and guided through them. Figure 7 shows the light coupling into a typical
Proc. of SPIE Vol. 6881 688114-7
F i b e r M o d e
W G M o d e
W G ( w r i t t e n w i t h a S l i t 1 . 5 m m )
S c a l e : m i c r o m e t e r s


waveguide using 633 nm laser from a He-Ne laser. Figure 7(a) clearly indicates the streak of light guided along the
waveguide whereas a small detuning of the laser beam path shows the streak vanishing indicating the light is now not
coupled demonstrating the absence of any waveguide [figure 7(b)]. Figure 8(a) shows typical mode profile of the output
from a fiber. Figure 8(b) shows image of the near field mode profile of a typical waveguide written using a slit of ~1.5
mm while scanning the sample at a speed of ~500 m/sec and an input energy of 30 J. The effect of the slit is clearly
seen in the figure 8(b) as the mode profile is fairly circular and comparable to fiber mode though it is bigger in size. The
mode profile obtained with waveguide written without the slit was indeed elliptical in nature. The profile of the
waveguide output clearly indicates single mode propagation. The loss measurements are in progress to determine the
parameters which favor the light propagation through these waveguides with minimum attenuation. The waveguides
having circular cross section are expected to possess lower losses as compared to the ones with elliptical cross sections.
There have been several recent studies
23-40
investigating the fabrication of waveguide lasers, microfluidic structures, and
Fiber Bragg gratings in variety of glasses. Baccarat glass is a potential glass in telecom spectral range and the possibility
of making passive photonic structures in these glasses along with the capability of LDW to fabricate photonic devices in
passive/active glasses augers well for the telecommunication applications. That the femtosecond laser pulses are able to
join two similar/dissimilar glasses
41
increases the opportunity of writing structures separately in passive and active
glasses and join them for a fully functional photonic device. Our future investigation will focus on the optimization of
writing conditions for enhanced waveguide performance and demonstration of amplification in these waveguide
structures.
Figure 8 Near field mode profile of the waveguides inscribed in baccarat (b and c) as compared to the fiber mode profile (a)
5. CONCLUSIONS
Gratings and waveguides were inscribed in Baccarat glass using the technique of femtosecond laser direct writing. The
change in refractive index was estimated to be of the order of 10
-3
. Micro-Raman measurements confirmed that there
was an increase in refractive index in the laser modified regions. By placing an appropriate rectangular slit before the
focusing microscope objective and by varying the sample translation speed and femtosecond laser energy waveguides
with circular cross-section were achieved. Measurements of the propagation losses are in progress and will be reported
else were. Baccarat glass is a material promising for fabrications of waveguides and other devices by LDW, especially
in the spectral region of telecommunications.
6. ACKNOWLEDGEMENTS
S. Venugopal Rao thanks the Department of Science of Technology, India for financial support through a SERC project
SR/S2/LOP-11/2005. D.N.R. and K.C.V. acknowledge the financial support from DST-ITPAR project. R.S.S.
Kumar acknowledges financial support from CSIR in the form of SRF.

(b)

(a)
Proc. of SPIE Vol. 6881 688114-8


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