Vol. 26, No.

23 | 12 Nov 2018 | OPTICS EXPRESS 29669

Femtosecond laser induced selective etching

in fused silica: optimization of the inscription
conditions with a high-repetition-rate laser
source
JIA QI,1,2 ZHENHUA WANG,3,4,6 JIAN XU,3,4 ZIJIE LIN,3,4 XIAOLONG LI,3,4
WEI CHU,1 YA CHENG,1,3,4,5,7
1State Key Laboratory of High Field Laser Physics, Shanghai Institute of Optics and Fine Mechanics,
Chinese Academy of Sciences, Shanghai 201800, China
2University of Chinese Academy of Sciences, Beijing 100049, China
3State Key Laboratory of Precision Spectroscopy, East China Normal University, Shanghai 200062,

China
4XXL–The Extreme Optoelectromechanics Laboratory, School of Physics and Materials Science, East

China Normal University, Shanghai 200241, China

5Collaborative Innovation Center of Extreme Optics, Shanxi University, Taiyuan, Shanxi 030006, China
6zhwang@phy.ecnu.edu.cn
7ya.cheng@siom.ac.cn

Abstract: Femtosecond laser induced selective etching (FLISE) of dielectric materials is a

promising technique for fabricating various microfluidic devices. Here we experimentally
studied the dependence of the selective etching speed in fused silica glass on laser pulse
energy, repetition rate, and inscription speed using a 1030 nm femtosecond laser. The
evolution of micromorphology of the laser inscribed lines was revealed with optical
microscopy, scanning electron microscopy, as well as anisotropic diffraction of the optical
gratings formed by these inscribed lines. A single pulse energy threshold is required to initiate
the FLISE. Further, a laser repetition rate window between an upper threshold and a lower
threshold was observed, which were limited by the thermal-induced disruption of the
nanogratings and by the disconnection of successive pulses modified spots respectively. The
synergetic influences of the above factors were evaluated by the exposure laser energy
density, which shows a common threshold for different inscription conditions and
demonstrates itself to be an excellent criterion for choosing appropriate parameters in FLISE.
The formation of continuous nanogratings is confirmed to be the major mechanism of FLISE
in fused silica. Our observations not only help one to understand the micro mechanism in
FLISE of fused silica, but also are of great use for fabricating large-scale microfluidic
circuits.

© 2018 Optical Society of America under the terms of the OSA Open Access Publishing Agreement

1. Introduction
Focused femtosecond laser radiation can induce highly localized modification in the chemical
and physical properties of transparent mediums allowing femtosecond laser direct/assistant
fabrication of various compact micro/nano structures inside the bulk materials [1–4], which
has paved the way towards a wide range of applications in three-dimensional (3D) photonics
integration [5–7], 3D microfluidic chips [8–10], micro mechanical elements and other
functional lab-on-a-chip devices etc [11,12]. Among the fascinating applications,
femtosecond laser-induced selective etching (FLISE) of transparent dielectric materials [13–
15] is a particularly interesting topic because of its important applications in the fabrication of
arbitrary 3D microfluidic, optofluidic and integrated multifunctional chips [10–12,16–18].

#345943 https://doi.org/10.1364/OE.26.029669
Journal © 2018 Received 14 Sep 2018; revised 18 Oct 2018; accepted 23 Oct 2018; published 29 Oct 2018
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29670

Due to its excellent physical and chemical stability and bio-chemical compatibility, fused
silica becomes the primary choice of the FLISE materials for microfluidic devices [17–19].
There are mainly two steps in the FLISE process of fused silica [13–15]. Firstly, the
femtosecond laser beam is focused into the glass substrate mounted on a motorized 3D
translation stage to inscribe desired patterns by moving the laser focus inside the material.
Due to some optical nonlinear effects including multiphoton absorption and localized plasma
excitation etc., only the laser-irradiated zones at the focus undergoes complex chemical and
physical properties modifications, which are much easier etched by hydrofluoric acid (HF)
[13–15] or potassium hydroxide (KOH) [20–23] than the surrounding material without laser
exposure. Secondly, the laser processed sample is immersed in the HF or KOH solutions to
selectively etch away the laser inscribed patterns and form hollow structures such as micro
tubes and cavities of the desired microfluidic devices.
The micro mechanism of the FLISE in fused silica glass is currently considered as the
chemical bonds break due to multiphoton ionization and the formation of self-ordered
periodic nanogratings resulted from local plasma micro-explosion of the ionized high-density
charges induced by the focused femtosecond laser beam [15,24–27]. The former loosens the
chemical structure of the glass and makes it easier to dissolve in HF or KOH solutions, while
the latter is beneficial to the penetration of the solutions inside the laser processed patterns
through these nanochannels due to capillary effect, and both greatly accelerate the chemical
etching speed of the laser inscribed patterns. However, the underlying physical and chemical
mechanism responsible for the FLISE has yet to be clearly understood.
The FLISE speed is essentially important in applications especially for fabricating large-
scale microfluidic devices, which is mainly determined by the etching agent and the laser
inscription parameters. Although HF solution was first used for FLISE of fused silica [13], it
is not a good choice for preparing uniform micro channels due to its relatively fast etching
speed to the non-irradiated materials, i.e., the etch rate between the modified and unmodified
materials is limited. Hot KOH solution is an excellent candidate for selective etching of fused
silica with the advantage of higher selectivity and lower harmfulness to human body, thus has
now become more and more popular [21–23]. Because the orientation of the femtosecond
laser-induced nanochannels is perpendicular to the laser polarization, rapid and uniform
selective etching can be achieved by tuning the laser polarization perpendicular to the
direction of the desired microfluidic channels or using circularly polarized laser beam in the
fabrication of arbitrary 3D microfluidic devices [25–29]. In addition, other laser parameters
including wavelength, pulse duration, pulse energy, and laser repetition rate as well as
fabrication conditions such as inscription speed also have very important influences on the
formation of the nanogratings [30–36] and the selective etching speed [15,20–22], which also
vary for other dielectric materials [37]. Nevertheless, the recent development of high
repetition rate, high average power femtosecond lasers has opened a new parameter space
which has been largely unexplored before. The optimization and refinement of FLISE will be
of particular implication because the high repetition laser sources can potentially provide
much greater fabrication throughput which will enable mass-production of large-scale micro-
devices with enhanced functionalities [20–22].
In this work, we systematically study the influences of the single pulse energy, repetition
rate and inscription speed on the FLISE speed in fused silica glass using an infrared
femtosecond laser at 1030 nm, and the transformations in micromorphology of the laser
inscribed region under different writing parameters are revealed using optical microscopy and
scanning electron microscopy (SEM). We also fabricate a series of optical gratings using the
same inscription parameters and non-destructively characterize the development of nano-
gratings by measuring the anisotropic diffraction of the optical gratings since the nanogratings
structure has remarkable optical anisotropy, which has been utilized to fabricate various
optical anisotropic devices [38–41]. We show that there exist a single pulse energy threshold,
a laser repetition rate window, and an exposure laser energy threshold in the process of
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29671

FLISE, and confirm that the main microscopic mechanism of FLISE is the formation of
continuous nano-gratings.
2. Experimental methods
The home-built 3D femtosecond laser modification setup is schematically shown in Fig. 1. A
regeneratively amplified mode-locked fiber femtosecond laser (Pharos 20W, Light
Conversion) operating at the wavelength of 1030 nm, a pulse duration of 290 fs and a pulse
repetition rate of 1MHz was used as the writing laser source. variable pulse repetition rate
ranging from 100 Hz to 1 MHz was used as the writing source. With a 0.3 numerical aperture
(NA) objective (Olympus, MPLFLN10x), the linearly polarized laser beam was focused 200
μm beneath the surface of polished fused silica plate sitting on a motorized 3D translation
stage. The fused silica plates were scanned perpendicularly to the propagation of the laser
beam with its polarization perpendicular to the scanning direction for best FLISE selectivity
and etching speed, as illustrated in the inset of Fig. 1. The laser pulse energy was adjusted
with a variable neutral density filter (VNDF), the pulse repetition rate was varied ranging
from 100 Hz to 1 MHz with a built-in acousto-optic pulse picker setting at the output port of
the laser system, and a coaxial microscope setup assembled with a CCD camera was used to
monitor the writing process.

Fig. 1. Experiment setup of 3D femtosecond laser modification system. VNDF: Variable

neutral density filer.

For selective wet-etching experiments, five parallel lines spaced by 50 μm were organized
into an array and each array was inscribed inside the fused silica plate with the same laser
modification conditions. After laser exposure, the end facets of the fused silica plate
perpendicular to the inscribed lines was polished to eliminate the boundary effect so that the
end faces of these modified lines were completely exposed outside. Then the specimens were
immersed in a chemical etching cuvette filled with KOH solution with a concentration of 8
mol/L and treated at a temperature of about 85 °C in an ultrasonic bath for 5 hours. After the
chemical etching and cleaning, the in-volume micro-channels were examined using a
transmission optical microscopy, and the lengths of the etched channels were measured to
calculate the selective etching speed. The data obtained under each modification conditions
were averaged over five measurements from the five lines in each array.
Another group of specimens was inscribed with the same modification conditions to
inspect the micromorphology of the laser modified channels by SEM. Differently, the top
surfaces of the plates perpendicular to the laser beam were polished so that the longitudinal
sections of the modified channels were exposed outside. Then the specimens were chemically
etched with the KOH solution for about 15 minutes so that the inner morphology can be well
imaged with SEM.
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29672

To non-destructively study the evolution of the femtosecond laser modification with the
change of the inscription parameters, a set of optical gratings with a period of 10 μm and a
total size of 3 x 3 mm2 were fabricated in identical fused silica plates with various writing
parameters, and the polarization of the laser beam was also perpendicular with the grating
lines as shown in the inset of Fig. 1. The optical gratings were probed with a linearly
polarized laser beam at the wavelength of 515 nm from normal incidence. The powers of the
first-order Raman-Nath diffraction light of the probe beams with different polarization
parallel (p) or perpendicular (s) to the grating lines were measured to calculate the diffraction
efficiencies, and the ratios of the 1st order diffraction efficiencies with different input
polarizations were used to characterize the anisotropy of the optical gratings.
3. Results and discussion
A typical transmission optical micrograph of a set of selectively etched micro channels
prepared by femtosecond laser with a single pulse energy of 2.0 μJ and an inscription speed of
1 mm/s using different pulse interval (TPI) or laser pulse repetition rate (Rrep) is shown in the
bottom of Fig. 2, where the parallel lines are the laser inscribed channels and the black lines
are the etched hollow microtubes. It is clearly seen that the selective etching can only occur at
a certain range of pulse interval (or laser repetition rate). Note that the pulse interval and the
laser pulse repetition rate are a pair of reciprocal parameters of each other, i.e., TPI = 1/Rrep.

Fig. 2. Transmission optical micrograph of selectively etched microchannels and the non-
etched lines inscribed by femtosecond laser with different pulse interval (laser repetition rate)
at a pulse energy of 2.0 μJ and an inscription speed of 1 mm/s.

As shown in the zoom-in pictures of the un-etched channels on top of Fig. 2,

microbubbles and weak re-vitrification zones are formed due to heat accumulation for Rrep = 1
MHz and 500 kHz (corresponding to TPI = 1 μs and 2 μs respectively), which interrupt the
connection of the laser-induced nanogratings [35,36] and thus break the selective etching
process. While when TPI ≥ 5000 μs, single laser pulse modified dots separate from each other
and no selective etching can occur. However, although the resulted etching speed varies as TPI
increases from 3 μs to 2000 μs, no clear difference in the un-etched channels’
micromorphology can be distinguished from the optical micrograph except for their widths.
The dependence of the FLISE speed on the inscription laser repetition rate (pulse interval)
with different pulse energy (Ep) and inscription speed (vc) is plotted in the left of Fig. 3, and
several properties can be seen from the experimental results.
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29673

1) There is a lower threshold of pulse energy Eth for FLISE at about 0.5 μJ, which
corresponding to a peak intensity of about 5.5 × 1013W/cm2. When the pulse energy
is lower than this threshold, selective etching can hardly occur since the laser
intensity is too low to induce necessary nonlinearity for generating the nanogratings.
2) There is an upper threshold of laser repetition rate (Rup) or a lower threshold of pulse
interval for FLISE limited by the heat diffusion speed. At high repetition rate (~1
MHz), local melting and re-vitrification of the glass will occur in the laser exposure
zone due to heat accumulation, which results in the formation of microbubbles
together with the destroy of the laser induced nanogratings [34–36,42,43] and thus
the interruption of the selective etching. As the accumulated heat is proportional to
the exposure energy, the Rup decreases from about 500 kHz to 200 kHz with the
increasing of the laser pulse energy from 0.75 μJ to 3.5 μJ.

Fig. 3. Left: Dependence of the selective etching speed on the laser repetition rate (or pulse
interval) with different pulse energy (Ep) and inscription speed (vc). Right: Replot of the FLISE
speed in the left data as the function of the exposure laser energy density Eden

3) There is also a lower threshold of laser repetition rate (Rlow) for FLISE depending on
the inscription speed and the pulse energy. The minimum repetition rate (Rmin) for
writing continuous structures is that the modified spots by successive pulses can
form connected lines, which can be calculated by Rmin = vc/deff, where deff is the
effective diameter of the single pulse modified spot. As the full width at half
maximum diameter of the laser beam at the focus (dFWHM) is about 2 μm in our
experiments, we have Rmin = 500 Hz for vc = 1 mm/s, Rmin = 2.5 kHz for vc = 5 mm/s,
and Rmin = 10 kHz for vc = 20 mm/s respectively, assuming deff = dFWHM = 2 μm. For
lower pulse energy (e.g., Ep = 0.75 μJ), the experimental results of Rlow are slightly
larger than Rmin, which means that multi pulses excitation is required in the lower
pulse energy case because the effective diameter filled with nanograting structures is
smaller than dFWHM due to nonlinear threshold effect, or the density of the single-
pulse induced nanograting is too low to be selectively etched. On the other hand, the
experimental Rlow for larger pulse energy (e.g., Ep ≥ 2.0 uJ) is smaller than Rmin
because the laser beam intensity outside of dFWHM is also strong enough to generate
high density nanogratings and the resulting deff is larger than dFWHM, which also
indicates multi pulse excitation are not necessary in the FLISE process. Accordingly,
the maximum inscription speed vmax for FLISE is determined by vmax = Rrep∙deff and
thus femtosecond laser system with higher repetition rate are much favorite to speed
up the fabrication of microfluidic devices by FLISE. Due to this limitation, the vmax
for FLISE of fused silica in our case can be up to 400 mm/s without heat
accumulation effect (Rup = 200 kHz) using a moderate pulse energy.
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29674

4) The selective etching speed is almost constant at about 280( ± 30) μm/hour between
Rlow and Rup for different pulse energies above the threshold Eth, although the widths
of laser inscribed lines vary with the repetition rates and the laser pulse energy as
shown in Fig. 2, which indicates that the selective etching speed is mainly
determined by the longitudinal micromorphology along the laser modified lines
rather than the transverse width of these lines. Since the normal etching speed of the
original fused silica substrate without laser modification (S0) is measured to be about
0.25μm/hour, such a selective etching speed results in an etching selectivity of about
1120( ± 120) defined by the ratio of the selective etching speed and the normal
etching speed S0, which is consistent with the results reported in [21] and is much
favorable for the fabrication of uniform and the precision of complex microfluidic
structures.
5) To evaluate the synergetic influences of the pulse energy, laser repetition rate as well
as the inscription speed, we replotted the FLISE speed as the function of the
exposure laser energy density Eden determined by Eden = Ep∙Rrep/(vc∙dFWHM), as shown
in the right of Fig. 3. Except for the case of Ep = 0.50 μJ which is around the single
pulse energy threshold, the minimum Eden for efficient FLISE (i.e., the lower
threshold of Eden) is almost identical at about 0.5 μJ/μm2 for different inscription
conditions, and then the selective etching speed is quickly saturated with the increase
of Eden. The upper threshold of Eden varies with the inscription speed, which is
determined by the laser repetition rate as discussed above. The identical lower
threshold of Eden (Edmin) indicates the laser modification process in FLISE is mostly
an energy accumulation effect, and demonstrates that the exposure laser energy
density Eden is a good criterion for choosing appropriate inscription conditions in the
fabrication of microfluid devices by FLISE. Accordingly, the maximum inscription
speed is also limited by v’max = Ep∙Rrep/(Edmin∙dFWHM) due to the requirement of the
minimum exposure energy density, and it is evaluated to be about 400 mm/s using Ep
= 2μJ, Rrep = 200 kHz and dFWHM = 2 μm respectively, which is equal to the result
evaluated using connected modification conditions discussed in context.

Fig. 4. SEM images of the femtosecond laser modified lines’ micromorphology inscribed with
different pulse repetition rate using fixed pulse energy of 2.0 μJ and inscription speed of 1
mm/s.

The SEM images of the femtosecond laser inscribed lines’ cross section perpendicular to
the laser propagating direction written with the same conditions as that for Fig. 2 are shown in
Fig. 4. For Rrep = 1 MHz and 500 kHz, due to heat accumulation and thermal diffusion, only
discrete nanostructures disperse in the laser inscribed lines surrounded by re-solidified melt
zones, which even seems chemical etching resistant seen from the SEM images. When Rrep
decreases to 333 kHz, clear nano gratings appear since most thermal energy due to single
laser pulse excitation can diffuse and relax into surrounding materials before subsequent pulse
arrives, but there are still some discrete melt zones that break the connection of these nano
gratings. With the further decrease of Rrep, only regular and connected nano gratings are
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29675

maintained in the laser inscribed lines with a gap width of about 300 nm as shown on the right
of Fig. 4, and the total width of the nanogratings across the laser inscribed lines also decreases
gradually, which is consistent with the optical microscopy results shown in Fig. 2. The single-
pulse-induced nanostructures are still clearly visible when the Rrep is reduced to 0.2 kHz, but
they are no longer connected with each other. By comparing with the SEM pictures shown in
Fig. 4 and the selective etching results shown in Fig. 2, it is confirmed that both the
generation and the connection of the femtosecond laser induced nanogratings are the core
mechanism of FLISE in fused silica.
The 1st order Raman-Nath diffractive efficiencies of a set of optical gratings probed with
p and s polarized beams are shown in Fig. 5(a), which were inscribed with different laser
repetition rate using a fixed pulse energy of 2.0 μJ and an inscription speed of 5 mm/s. Due to
strong thermal diffusion effect at high Rrep, the width of the refractive index change region is
much larger than that of the laser focus, and the index change regions of the adjacent lines in
the optical grating overlap with each other. Therefore, although the refractive index change
can be large, the periodic modulation of the refractive index is very weak, and thus the
diffractive efficiencies is low for Rrep = 1 MHz and 500 kHz respectively. With the decrease
of Rrep, the refractive index change region gets narrower and the periodic modulation effect
gets stronger, so the refractive efficiencies of both the s and p polarized probe increases
gradually with the decrease of Rrep from 1 MHz to about 100 kHz. Meanwhile, the amplitude
of the periodic index modulation (i.e. the refractive index change) decrease with the decrease
of Rrep, thus the diffractive efficiency drops down again with the further reduction of Rrep.

Fig. 5. (a) 1st order Raman-Nath diffractive efficiencies of the optical gratings inscribed by
femtosecond laser with different repetition rate and probed with p and s polarized light
respectively. Inset: Illustration of the readout configuration and the Raman-Nath diffraction of
the optical grating. (b) Anisotropy of the optical grating comparing with the selective etching
speed of FLISE tubes prepared with the same inscription conditions.

The optical gratings’ anisotropy was evaluated by the ratio of the 1st order Raman-Nath
diffractive efficiencies for p and s polarized probes (ηs/ηp), and its dependence on the laser
repetition rate is shown in Fig. 5(b). It can be seen that the anisotropy is very small for the
gratings written with high repetition rate at 1 MHz, which is resulted from the erase of the
nano gratings due to thermal-induced melting. With the decrease of Rrep, the anisotropy of the
gratings ηs/ηp increases quickly from ηs/ηp ≈1.1 for Rrep = 500 kHz to ηs/ηp ≈1.7 for Rrep = 200
kHz and then decreases gradually to ηs/ηp ≈1.0 for Rrep = 1 kHz, which is consistent with the
SEM observations that the nano-gratings started surviving for Rrep = 500 kHz, and the density
of the nano-gratings increases and then decreases gradually with the decrease of the laser
repetition rate. By comparing the optical gratings’ anisotropy with the FLISE speed of the
micro tubes prepared with the same inscription conditions as well as the SEM observations, it
 Vol. 26, No. 23 | 12 Nov 2018 | OPTICS EXPRESS 29676

is further confirmed that the formation of the nano-gratings is the common mechanism of the
optical anisotropy and FLISE. It should be noted that we only discussed the longitudinal
etching speed along the nano-gratings and the laser-inscribed tubes, thus no influence of the
nanogratings’ density to the selective etching speed was observed.
4. Conclusions
In summary, we have systematically investigated the dependence of the FLISE speed in fused
silica on the inscription parameters including laser pulse energy, repetition rate and
inscription speed with a 1030 nm near infrared femtosecond laser. Optical microscopy,
scanning electron microscopy and anisotropic diffraction methods were adopted to reveal the
micromorphology of the femtosecond laser inscribed structures and thus the underlying
mechanism of FLISE. We confirmed that the formation of linked nanogratings is the main
mechanism of FLISE in fused silica. We showed that there exists a threshold of single pulse
energy Eth or a threshold of peak intensity to initiate the FLISE. With a pulse energy above
Eth, there exists a laser repetition rate window for FLISE between an upper (Rup) and a lower
(Rlow) thresholds, where a constant etching speed of about 280( ± 30) μm/hour was achieved
with the pulse energy ranging from 0.75 μJ to 3.5 μJ using an inscription speed of 1 mm/s, 5
mm/s and 20 mm/s respectively. The upper repetition rate threshold is limited by thermal
diffusion and thus the local melting and re-vitrification effects of the glass at higher laser
repetition rate, while the lower threshold is determined by the inscription speed and the
effective diameter of the single-pulse-modified spot, indicating higher repetition rate
femtosecond laser system are favorite to speed up the FLISE and the fabrication of
microfluidic devices. The synergetic influences of the pulse energy, laser repetition rate and
the inscription speed were expressed by the exposure laser energy density Eden, which shows a
common threshold for different inscription conditions and demonstrates itself an excellent
criterion for choosing appropriate inscription conditions in the fabrication of microfluidic
devices by FLISE. Our result will have important implication for fabrication of large-scale
microfluidic circuits and micromechanical devices.
Funding
National Key R&D Program of China (2018YFB0504400), National Natural Science
Foundation of China (11874154, 11734009, 11674340, 61590934, 61675220, and 61505231),
Strategic Priority Research Program of the Chinese Academy of Sciences (XDB16030300),
Key Research Program of Frontier Sciences, Chinese Academy of Sciences (QYZDJ-SSW-
SLH010), Project of Shanghai Committee of Science and Technology (17JC1400400), and
Shanghai Rising-Star Program (17QA1404600).
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