Optics & Laser Technology 179 (2024) 111337

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Optics and Laser Technology

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Nanosecond laser induced periodic silicon microstructures for broadband

antireflective applications
Albin Kuriakose a, b , Pariksha Malik b , Jitendra Nath Acharyya a, 1 , Dinesh Kalyanasundaram c, d ,
Pankaj Srivastava b , G. Vijaya Prakash a, *
a
Nanophotonics Lab., Department of Physics, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India
b
Nanostech Lab., Department of Physics, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India
c
Centre for Biomedical Engineering, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India
d
Department of Biomedical Engineering, All India Institute of Medical Sciences, Ansari Nagar, New Delhi 110016, India

A R T I C L E I N F O A B S T R A C T

Keywords: Laser-driven micro/nano-texturing is a remarkably efficient and cost-effective technique, having diverse appli­
Silicon microstructures cability in the realm of photonics, optoelectronics, and photovoltaics. Here, we demonstrate the high-intensity
Nanosecond laser texturing nanosecond laser-matter interactions for periodic micro/nanostructures on silicon, exclusively to emphasize
Laser-matter interaction
the effects of laser parameters for large-scale integration. A wide range of periodic structure rapid fabrication
Large-scale fabrication
Broadband antireflective structures
over a wafer level is systematically studied for optimised parameters using nanosecond laser pulses (1064 nm,
50 ns) at different pulse repetition rates ranging from 10 to 40 kHz. A comprehensive understanding based on
physical, structural, and optical studies reveals a strong correlation between the formation of nano/micro­
structure morphology and the laser parameters. The laser-matter interactions result in trench-like periodic
patterns, formation of nanostructure agglomerations as light-trap-centres on the silicon surface. Such nano/micro
periodic structures provide a dominant reduction in reflection losses of up to 80 % over a broad UV-NIR spectral
region. The studies further demonstrate that the periodic structural patterns could also be potentially utilised for
large-scale optical diffraction applications. In addition, the extra layer coating of Silicon Nitride (Si3N4) on the
textured silicon further reduces the reflection losses, which is an added advantage of integrated silicon tech­
nology. The present work could open a commercial pathway for the rapid fabrication of nanosecond laser-based
nanotexturing and periodic grating structures, enabling significantly reduced reflection and improved light
trapping in large-scale Silicon-based applications due to its speed, repeatability, and high precision.

1. Introduction efficiency [10]. For such applications, the bare silicon is typically
patterned by lithography [11], followed by conventional etching tech­
Micro- and nanotexturing of material surfaces for prospective uses in niques including reactive ion etching, plasma etching, or chemical
MEMS devices [1], reduced reflection [2,3], increased absorption, etching [12,13]. The most common methods typically rely on mask
modulation of wettability [4–6], etc., have engendered keen interest copying, rendering them less flexible and adaptable for pattern gener­
among researchers in the past decade. The prior texturing of silicon is ation. The direct patterning techniques offer enhanced versatility over
required for specific applications in semiconductor devices, namely, conventional multi-step patterning methodologies. Among them, laser
solar panels, microsystems, and integrated circuits [7–9]. This is due to direct writing is a one-step process that is highly beneficial for achieving
the fact that the efficiency of light collection and absorption is poor precise patterning with satisfactory surface qualities for large-scale
because of the high reflectivity of bare and polished silicon in the visible integration. Pulsed lasers, such as nanosecond lasers, are often
and NIR spectral regions. Nano- and micro-structuring on silicon sur­ employed for rapid and cost-effective surface texturing of diverse sur­
faces has been routinely performed to achieve low-reflecting silicon face morphologies resulted by complex laser-matter interactions
surfaces (known as black silicon) for enhanced light absorption [14–16]. Over the past decade, laser processing and laser-based

* Corresponding author.
E-mail address: prakash@physics.iitd.ac.in (G. Vijaya Prakash).
1
Currently at LP2N Laboratory, Institut d’Optique Graduate School, Université de Bordeaux, 33400 Talence, France.

https://doi.org/10.1016/j.optlastec.2024.111337
Received 3 December 2023; Received in revised form 10 June 2024; Accepted 12 June 2024
0030-3992/© 2024 Published by Elsevier Ltd.
A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

structuring [17] have established significant strides in altering the sili­ The optical microscope, SEM, FESEM, and AFM were employed to
con’s surface morphology [18] and enhancing the light absorption/ visualize the surface morphology of the fabricated samples. Reflection
trapping capabilities [19]. The silicon surface texturing during pulsed spatial spectral mapping was carried out by the modified optical mi­
laser interaction can be selectively controlled by the laser parameters croscope coupled to a spectrometer and Xenon/DI lamps. The conven­
such as pulse width (femto-, pico-, nano-second and CW), laser fluence, tional reflection spectra were recorded on a commercial UV–VIS-NIR
repetition rate (few Hz to MHz), etc. [20–23]. The laser surface crys­ spectrophotometer by keeping the c-Si as the reference. Multiple-
tallisation process [24,25] and laser-induced periodic surface structures aperture diffraction experiments were performed with a 405 nm laser
ranging from several microns down to a few hundreds of nanometers and the diffraction patterns were recorded using a computer-controlled
[26–28] emerge on the material surface because of the various laser- motorised stage coupled to a photodetector. The diffraction beam spatial
induced material modification effects. The shapes and orientations of profiles were also captured using a beam profiler. An additional stoi­
laser-induced structures have been found to be influenced by several chiometric silicon nitride (Si3N4) layer of ~ 150 nm was coated on the
processing factors, including laser fluence, the quantity, length, and structured silicon substrates using plasma- enhanced chemical vapour
polarization of the laser pulses [29–32]. Laser texturing and ablation of deposition (PECVD) technique.
wide variety of materials are not only dependent on the material char­
acteristics but also critically dependent on various laser parameters such 3. Results and discussion
as pulse width, repetition rate, scanning speed, laser fluence, polar­
isation, laser beam spot size/shape, etc. Several attempts are being made The laser texturing on the silicon wafer has been carried out using a
to model the characteristic features of laser-induced nano/micro tex­ commercial nanosecond laser (1064 nm, 50 ns) with a variable pulse
tures. Analytical models utilise pulsed laser parameters, such as gaussian repetition rate of from 10 kHz to 40 kHz and a maximum average power
spatial beam profile overlapping and/or pulse-to-pulse overlapping of 50 W with an automated XYZ laser head/sample stage (Fig. S1).
during the laser-matter interaction leading to femto/picosecond laser- However, the average power substantially varies with the laser repeti­
based photothermal processes to optimize the fabrication speed and tion rate (pulse-to-pulse duration) (see Fig. S2). A series of experiments
size/depth of nano/microstructures [33,34]. Specifically, the modelling were carried out for various laser pulse repetition rates upto 100 kHz
of femto/picosecond laser-matter interactions in metals and metal alloys and it was found that under 40 kHz, the silicon wafer sustains the
typically follow analytical models, based on fluence and pulses-per-spot physical laser damage or breakage. Since the nanosecond laser-based
(F-PPS) and accumulated fluence profile (AFP) to predict, reproduce and engraving instrument is a commercial instrument that is widely uti­
control the desired textures [35,36]. Few mathematical models are also lized for various mechanical, optoelectronic, and biomedical applica­
being employed in metal alloys to understand the nanosecond laser tions, we can achieve selective texturing of the silicon surface for rapid
surface texturing processing strategy and reproducibility of different and large-scale fabrication [38–40].
shape and sized micro patterns [37]. In general, it is utmost important to The periodic laser texturing was performed at constant laser power
delve into a comprehensive study of laser structuring across different with a fixed spot size at the focus of 30 μm. During this comparative
pulsed (nano, pico and femtosecond) lasers and varieties of materials, as study, we fixed the laser repetition rates at 10 kHz, 20 kHz, and 40 kHz.
the nature of laser-matter interaction varies in accordance with the The periodic laser texturing on silicon wafers at 10 kHz, 20 kHz, and 40
fundamental laser parameters. kHz repetition frequencies with pattern pitches of 40 μm, 30 μm, and 20
In this present work, the nanosecond laser interaction with silicon at μm is systematically performed and studied. The detailed surface
various laser repetition rates has been explored to selectively texture the morphology of the laser-textured samples was characterized by optical
silicon surface for rapid and large-scale fabrication. The comprehensive and electronic (SEM, FESEM) and atomic force (AFM) microscope im­
study reveals how the fabricated micro/nano structures collectively help ages. The SEM and optical microscope images of the laser-patterned Si
to enhance the antireflection and the absorption capabilities. The laser substrate at three different pulse repetition frequencies are shown in
texturing was performed in grating type vertical lines with different Fig. 1. Other studies for different laser power levels at 20 and 40 kHz
periodicities for different repetition rates of the nanosecond laser. The repetition rates and various scan speeds (1 mm/s to 1000 mm/s) at fixed
micro- and nanostructures formed during laser patterning act as light- 10 kHz repetition rate are shown in Fig. S3 and S4, respectively. As
trapping centers and increase the absorption capability of the silicon observed in Fig. 1(a-c), the samples fabricated at a 10KHz repetition rate
substrate. In addition to the above, the presence of an anti-reflecting exhibit ripple-like structures. As the pitch decreases, the lines become
coating (a stoichiometric silicon nitride (Si3N4) layer) brings a drastic closer together, and at a pitch of 20 μm, the lines almost overlap with
reduction in the reflection losses. each other. At higher pulse repetition rates, such as 20 kHz (Fig. 1(d-f))
and 40 kHz (Fig. 1(g-i)), the laser trench appears wider, causing more
2. Experimental section damage compared with the 10 kHz laser pulses due to the cumulative
heating effect experienced by the Si substrate. In almost all samples, the
Fabrication of microstructures was carried out on a p-type silicon debris formation is most dominant at higher repetition rates. The vari­
wafer (1 0 0) using Markolaser customized commercial laser writing for ation in the laser patterning and the interaction of nanosecond laser
large-scale and mass production. Infrared nanosecond laser (1064 nm, pulses with the silicon substrate for different repetition rates were
50 ns) repetition frequencies were optimised for the variation from 10 evident from the SEM and optical microscope images. As an example,
kHz to 40 kHz at the same average power levels. For more than 40 kHz the large wafer-scale laser patterned texturing is also shown in Fig. 1 for
pulse repetition rates, the substrate damage has been observed. A laser one of the optimized parameters (10 kHz, 30 μm gap).
beam spot size of 30 μm was used for writing, utilizing galvo-mirrors for The observed ripple-like structures and the formation of nano- and
writing gaps of 40 µm, 30 µm, and 20 µm. The scan speeds were varied micro-structures in the SEM and optical images are further closely
from 1 mm/s to 1000 mm/s and for optimised results, the laser scan observed using FESEM measurements. These structures along the laser
speed was kept constant at 10 mm/s. A schematic diagram of the written areas resulted from various complex laser-matter interaction
experimental setup is shown in Fig. S1, and the laser optimisation for mechanisms. Fig. 2 displays various magnifications of the FESEM images
different peak powers and pulse frequencies is shown in Fig. S2. Opti­ for laser-patterned Si substrates at various pulse repetition rates. The
mization of laser parameters such as peak power for various repetition formation of nano agglomerated particles at higher repetition rates (at
rates and various scan speeds are done before the experiments (see 20 kHz and 40 kHz) are more pronounced as compared to the low
Fig. S3 and Fig S4). Before and after the laser patterning, the samples are repetition rate (at 10 kHz). At 20 kHz (Fig. 2(b)) and 40 kHz (Fig. 2(c))
ultrasonically cleaned using DI water and propanol, followed by a 20 % laser repetition rates, one can observe the increased accretion of the
HF solution to remove any native oxide layer. nanostructures as a cluster in the patterned line and in the gap between

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A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 1. SEM and optical microscope images (in false colour) of laser-patterned Si substrates at three different pattering pitches of 40, 30, and 20 μm, as well as for
laser pulse repetition rates (a-c) 10 kHz, (d-f) 20 kHz, and (g-i) 40 kHz. Bottom camera images (with optical microscope close-up images as inset) demonstrate the
large-scale rapid fabrication over a silicon wafer (10 kHz, 30 µm gap). The nanosecond laser parameters are 1064 nm wavelength, 50 ns pulse width, and a beam spot
size of 30 μm.

these laser trenches. The average particle size distribution histogram images, and reflection spatial mapping has been carried out and re­
plots suggest typical average sizes of 30–60 nm with increasing trend ported in Fig. 3. The large-area SEM, optical microscope images, and
with laser pulse repetition rate. The strong X-ray diffraction of laser reflection spatial spectral mapping of the periodic laser-textured silicon
written area suggests that the nanoparticles of polycrystalline nature is shown in Fig. 3(a-c). The reflection spatial spectral mapping of the
(Fig. 2(d)). The strong X-ray diffraction peaks in the laser written area textured silicon indicates a substantial reduction in the reflection loss in
suggest the nanosecond laser-induced localised crystallisation process. the patterned area. A close look at the individual laser-written trench
[24,25]. further offers a profound insight into the reflective losses and
Nanoparticle/debris agglomeration in silicon is known to increase morphology. The FESEM, AFM, and optical microscope images, along
the absorption and huge reduction in the reflectivity of the textured with the reflection spatial map of individual trenches are provided in
silicon (known as black silicon) [41]. The nanostructure formation Fig. 3(d-g). From the spectral reflection imaging, we can observe that
during the laser micromachining could possibly be visualised as photon each textured area plays an important role in reducing the reflection
trap centers with enhanced absorption and a substantial reduction in intensity of the broad-band white-light spectrum. A ripple-like structure
reflection loss of the material by exploiting the antireflection property of formation along the laser track is observed due to the overlapping of
the black silicon. Results suggest that the formation of nanoparticle consecutive laser pulses, possibly due to a mismatch between the speed
aggregation and trap nanocavities during the laser interaction are highly of the laser pulse train (scan speed rate), laser spot overlap, and pulse
dependent on the number of laser pulses per second experienced by the repetition rate. However, such macroscopic ripples are not obviously
silicon wafer. This has been experimentally demonstrated with variation observable during the optical reflection probing, and the resultant
of repetition rates and scan speeds (Fig. 1 and Fig S4). The thermal reflection loss within the single trench is about 30 % (Fig. 3(g)). These
energy dissipation into the silicon lattice at higher repetition rates (>20 results broadly reveal reduced reflection losses along the laser track
kHz) was found to be higher due to the large number of laser pulses compared to the normal smooth polished silicon substrate, which is a
interacting with the silicon at a given interval of time, resulting in the favourable result for many applications. The large-scale AFM images
predominant nanoparticle and structure formation in silicon. A detailed also reveal that the RMS surface roughness on the peripheral of the laser-
explanation of the effect of pulse repetition rate variation on laser- written area is about 120 nm (Fig. S5), which contains agglomerated
matter interactions has been discussed in the later section. nanoparticles as demonstrated in Fig. 2. The aforementioned results
To explore further deeper into the laser pattered area, a closer look at broadly indicate that the significant reduction in reflection loss along
the laser-written area from SEM, FESEM, AFM, optical microscope the laser pattern areas is caused by increased surface roughness and the

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A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 2. FESEM images at different magnifications of laser-induced surface nano/microstructures on Si substrate for samples at laser pulse repetition rates (a) 10 kHz,
(b) 20 kHz, and (c) 40 kHz, along with their respective Gaussian profile particle size distribution histograms. (d) XRD patterns of the micro/nanocrystal area of laser-
textured silicon along with standard c-Si powder and bare Si wafer. The nanosecond laser parameters are 1064 nm wavelength, 50 ns pulse width, and a beam spot
size of 30 μm.

formation of agglomerated nanoparticles. that with the increase in pulse width (in the picosecond regime), the
In general, the large-scale periodic patterning could be visualised as lattice temperature increases, which eventually controls the laser-
surface gratings for many light trapping and confining applications such written structure shape and size [45]. During a femtosecond laser-
as photovoltaic cells. Furthermore, to quantify and correlate the silicon interaction [46], the increase of nanoparticle debris and plume
experimentally obtained periodicity (pitch) of the laser-induced pat­ shield is observed up to a 10 kHz pulse repetition rate [47]. Similarly,
terns, typical laser diffraction measurements were performed on various the depth of picosecond laser writing decreases with the laser repetition
samples. The diffracted signal intensity was scanned along the length by rate due to the dominant shielding of debris and ablated particles [48].
a photodetector and the signal was also spatially mapped by the beam The dynamic and cumulative heat dissipation is one of the important
profiler (Fig. 4). Considering the Fraunhofer propagation criterion, the aspects of laser-matter interaction and particularly influences the laser
diffraction spatial intensity distribution can be represented as [42], written quality and laser − written pattern size and shape. Several laser-
( ( ))
matter interaction studies are reported on semiconductors and metals
I(x) = |E|2 1 +cos 2πλLΛx , where |E|2 is the far field intensity, λ is the
based on a wide range of laser characteristics features (beam shape and
wavelength of the laser, Λ is the pitch of the periodic pattern, L is the size, wavelength, pulse width (CW, fs, ps, ns) etc). Kanaujia et. al studied
distance between the sample and the detector. femtosecond laser-matter interactions and specially the shape and size
The variation in the distances between the patterns is evident from of laser engraved structures, which are dominated by chemical modifi­
the diffraction intensity and fitted parameters (pitch), which are in good cation followed by material ablation. It is also demonstrated that the
agreement with the parameters obtained from SEM and optical micro­ laser-matter interaction is dominated by high-density plasma genera­
scope images. These parameters, thus obtained with detailed compari­ tion, apart from other laser induced optical nonlinearities [49]. In
son, are summarized in Table 1. Due to the overlapping of the another work, Parmar et al. demonstrated that the nano scaffolding of Si
consecutive laser patterns, the diffraction intensity pattern was not surfaces induced by the femtosecond laser-matter interaction within the
observed for the samples fabricated at higher pulse repetition rates with liquid medium produces nano scaffolding from various concurrent
a low pitch. It is also to be noted that, as of today, very limited reports processes of photon absorption, electron–phonon relaxation induced
are available on nanosecond laser-based periodic patterns, and such lattice heating, material melting, and phonon–phonon relaxation
reports are either for a limited area or inscribing within the material induced cooling [50]. On the other hand, Parmar et. al have demon­
[43,44]. strated the investigation of heat dissipation and consequent micro
The effect of the variation in laser repetition rates in controlling the texturing of metals and metal alloys utilising nanosecond and CW fiber
formation of micro/nano structures is strongly dependent on the inter­ lasers. [51–53]. However, the nanosecond laser interaction and exclu­
action of the nanosecond laser pulse with the target material and it sive focus on the role of pulse repetition rate are not yet known, which is
depends upon various laser parameters, such as pulse width, pulse very essential for large-scale commercial-level laser patterning.
repetition rate, laser average power, etc. Previously, it was proposed It is evident that as the pulse repetition rate increases, the time in

4
A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 3. Large area laser-encrypted patterns captured by (a) SEM, (b) optical microscope (μscope) images, and (c) reflection spatial spectral mapping along with the
line profiles across the textured area for a 10 kHz repetition rate (pitch: 40 μm). A close view of an individual laser encryption of a single line pattern of (d) FESEM,
(e) AFM, (f) optical microscope images, and (g) reflection intensity spatial mapping along with X and Y line scans.

terval between (1/f) two consecutive laser pulses decreases, resulting in material. During the laser-material interaction, electron-hole pairs are
an increased cumulative and dynamic heating effects experienced by the produced in silicon by the incident laser energy. The thermal energy
target material. Since the laser pulse train travels at a constant speed (10 thus imparted on the bulk material is transferred to the lattice by the
mm/s), the repetition rate plays an important role in controlling the electron–phonon interactions. Since the nanosecond pulsed laser has a
interaction. The thermal diffusion coefficient of silicon is ~ 1.0 cm2/s, duration of 50 ns, which is longer than the electron–phonon relaxation
and the diffusion length depends on this coefficient along with the laser time (τe-ph – 260 fs) [57], silicon absorbs the complete energy and leads
parameters like repetition rate, pulse duration, and laser average power to the rise in temperature at maximum value at the end of the laser pulse.
[54]. The thermal diffusivity of silicon, which accounts for the tem­ The thermal diffusion length depends on the thermal diffusion coeffi­
perature dependency [55], can be expressed as D(T) = 1+aT DR
, where DR is cient of the material and the pulse duration according to the relation
( )1/2
the diffusion coefficient of silicon and a = 0.0072/ C. It is important to
◦
αd τ p . Because of this dependency, compared with femtosecond and
note that the laser-matter interaction is influenced by the material’s picosecond laser pulses, the nanosecond laser will induce more thermal
properties, with the dominant factor being the rise in material surface diffusion length for a material that is interacting with the laser pulse
temperature. When the speed of the laser track is significantly smaller [58]. During the laser matter interaction, the material gets evaporated
than the pulse repetition rate, multiple laser pulses interact in a specific and can form a thin layer of dense plasma plume. The plasma thus
area of the sample. Consequently, even when the laser power and laser formed can partially shield further interaction of the laser pulse with
track speed are kept constant, the interaction of the laser is primarily target material by absorbing energy from the laser pulse, which leads to
modulated by altering the pulse repetition rate, as supported by our an increase in the temperature and pressure of plasma [57]. A
results. phenomenological schematic plot of the temporal behaviour of the
For higher repetition rates, the incubation effect increases due to temperature rise or heat transferred for three different laser repetition
heat accumulation, which reduces the ablation threshold [56]. The heat rates is shown in Fig. 5. The pulse width of the nanosecond laser used for
accumulation during laser processing at different repetition rates de­ the present texturing is 50 ns, and during this time interval, it can be
pends on the heat capacity and thermal conductivity of the interacting speculated that the Si substrate gets heated rapidly and reaches

5
A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 4. Laser-written surface grating properties on Silicon. Diffraction intensity plots with varied pitches of (a) 40 μm, (b) 30 μm, and (c)20 μm using 10 kHz
repetition laser pulses (1064 nm, 50 ns). (d-f) are the respective 2D laser diffraction beam profiler images with 405 nm laser irradiation. Insets are the camera images
of the laser diffraction.

maximum temperature. Subsequent cooling of the substrate occurs

Table 1
during the interval of two consecutive pulses. The detailed morpho­
A summary of the expected and experimentally obtained pitch (Λ) of the peri­
logical study of laser patterning indicates that due to the enhanced heat
odic laser patterns for various samples. Laser parameters (1064 nm, 50 ns, 30 µm
accumulation at higher pulse repetition rates, a significant amount of
spot size, scan speed 10 mm/s).
silicon melts, resulting in molten and resolidified silicon on the surface.
Samples Repetition Laser-induced pattern Pitch (Λ) Estimate
For a low repetition rate (10 kHz), molten resolidified silicon produces
rate
in kHz
Expected From From From ripple-like structures that are periodic but have very little damage and
microscope SEM diffraction surface roughness.
images images patterns
±2 µm ±1 µm
The nano-traps and the periodic textures potentially influence the
reflection properties of silicon, as we can observe from Fig. 6(a-c), which
F10_40 10 40 µm 42 µm 43 µm 38 µm ± 1.3
shows the dominant reduction in the reflection losses of the silicon wafer
µm
F10_30 10 30 µm 32 µm 33 µm 32 µm ± 0.3 after nanosecond laser texturing with different periodicities using three
µm pulse repetition rates of 10 kHz, 20 kHz, and 40 kHz. The reflection
F10_20 10 20 µm 21 µm 22 µm 19 µm ± 0.7 spectral measurements have been done with silicon as the reference, so
µm the silicon reflection is shown as 100 % in the graphs (Fig. 6). More than
F20_40 20 40 µm 43 µm 43 µm 43 µm ± 0.5
µm
50 % reduction in reflection losses is observed at 10 kHz pulse repetition
F20_30 20 30 µm 34 µm 33 µm 35 µm ± 0.2 rate laser patterns. The reflection losses are further reduced with the
µm decreasing pitch of the periodic laser patterns. The laser-textured silicon
F20_20 20 20 µm − − − wafers at higher pulse repetition rate (20 kHz and 40 kHz) exhibit an
F40_40 40 40 µm 43 µm 43 µm 44 µm ± 1.8
even more prominent reduction in reflection loss (>70 % for 20 kHz
µm
F40_30 40 30 µm − − − samples and > 80 % for 40 kHz samples) with decreasing periodicities of
F40_20 40 20 µm − − − the patterns. The predominant reduction in reflection loss can be
attributed to the increased number of nanoparticles/nanostructures

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A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 5. A phenomenological model of nanosecond laser interactions and temporal heat dissipation. A schematic view of the temperature/heat dissipated during the
laser pulses at different laser pulse rates (a) 10 kHz, (b) 20 kHz, and (c) 40 kHz falls within the material. Corresponding SEM images of patterned silicon at different
laser pulse rates.

formed during the laser-silicon interaction at higher pulse repetition explored nanosecond laser-based engraving instrument. As discussed in
rates. the initial section (see Fig. 1), we have demonstrated experimentally a
To achieve further reduction in reflection loss, Si3N4 is deposited on large-scale nano/micro-structuring by laser texturing on a two-inch
top of the laser-textured silicon substrate. Owing to the wide trans­ silicon wafer. Since the instrument used for the fabrication is a com­
parency in the visible and NIR regions, Si3N4 is widely utilized for mercial and fully motorized programmable setup, we easily attain the
photovoltaic applications as a potential anti-reflective coating [59–61]. goal of large-scale production. The nanosecond laser parameters can be
The reflection spectra of the patterned silicon substrates with Si3N4- further optimized for better and more advanced nano- and micro-
coating are shown in Fig. 6(d-f), which shows further reduction in the structuring, which can be used for various photonics and optoelec­
reflection losses as compared to the stand-alone textured silicon sub­ tronics applications. The laser structuring for the antireflection appli­
strate. However, the coating of Si3N3 (~150 nm) provides an obvious cation can be recommended due to the possibility of large-scale
interference effect, which appeared as an oscillation pattern in the texturing for the commercial solar cell.
reflection spectrum of the conjugate system. The observed oscillations in
the reflection spectra of Si3N4-deposited samples can be attributed to the 4. Conclusions
formation of an oxide layer and non-uniformity during the deposition.
Laser texturing for reducing the reflection losses of the silicon sub­ In summary, the present study illustrates the rapid and large scale
strate for various photonic applications was demonstrated using the less wafer-level fabrication of optimised periodic structures on silicon using

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A. Kuriakose et al. Optics and Laser Technology 179 (2024) 111337

Fig. 6. Reflection spectra of patterned silicon substrates and Si3N4 coated on the top of such patterned substrates for three pulse repetition rates of (a,d)10 kHz, (b,e)
20 kHz, and (c,f) 40 kHz.

nanosecond laser pulses (1064 nm, 50 ns). The interaction of nano­ editing, Methodology. Jitendra Nath Acharyya: Writing – review &
second laser pulses with silicon at different laser pulse repetition rates editing, Methodology, Investigation, Formal analysis. Dinesh Kalya­
(from 10 to 40 kHz) was investigated to comprehend how the formation nasundaram: Writing – review & editing, Validation, Resources, Project
of micro- and nanostructures effectively enhances the antireflection administration, Methodology, Investigation, Funding acquisition,
properties through a cost-effective, simple, and scalable laser texturing. Formal analysis. Pankaj Srivastava: Writing – review & editing, Vali­
The study further reveals the mechanism of micro- and nanostructures dation, Supervision, Resources, Project administration, Methodology,
formation during laser-silicon interaction can be effectively tailored Funding acquisition, Formal analysis, Conceptualization. G. Vijaya
from controlled laser parameters such as pulse duration, scan speed, Prakash: Writing – review & editing, Writing – original draft, Visuali­
peak power, repetition rate. The silicon nano polycrystalline structures zation, Validation, Supervision, Software, Resources, Project adminis­
formed during the laser writing process revealed a broad size variation tration, Methodology, Investigation, Funding acquisition, Formal
from 35 to 60 nm, depending on the laser repetition rates. The rate of analysis, Data curation, Conceptualization.
laser pulse interaction is clearly visualised from the heat accumulation,
which is strongly dependent on material quantities namely, heat ca­
Declaration of competing interest
pacity, thermal diffusion, and thermal conductivity. The eventual laser-
material interactions are resulting into varieties of nano/micro­
The authors declare that they have no known competing financial
architectures that strongly enhances light trapping and absorbing
interests or personal relationships that could have appeared to influence
mechanism. The substantial reflection losses have been found with the
the work reported in this paper.
increase of train of nanosecond pulses (of > 25 µs) which is longer than
the electron–phonon relaxation times of silicon. A prominent reduction
Data availability
of reflection loss over 80 % in the broad spectral band (300–800 nm)
reflection spectra was achieved with laser-patterned silicon compared to
The data supporting the findings of our study can be found in the
the conventionally polished silicon. This reduction can be attributed to
article and the supplementary information.
the enhanced broadband light absorption capabilities exhibited by the
agglomerated silicon nanoparticles or micro/nano structures (light
Acknowledgements
trapping centers) formed during the laser processing. For further device
application point of view, the additional Si3N4 coating on laser textured
Authors acknowledge Central Research Facility (CRF) (funded by
silicon can further enhance the reflection losses as compared to the
Government of India), Indian Institute of Technology (IIT), Delhi for
pristine textured silicon. Broadly, the proposed knowledge of nano­
providing FESEM facility and AFM Lab, Department of Physics, IIT
second laser texturing is a fast, cost-effective, and reliable method for
Delhi. AK, PM and JNA acknowledge IIT Delhi, UGC (Govt of India) and
large-scale manufacturing, which could possibly be potential for the
DST-Inspire (Govt of India) for Research Fellowship. Sonu Singh for
prefabricated optoelectronic and photovoltaic devices.
support with nanosecond laser operation is acknowledged.
CRediT authorship contribution statement
Appendix A. Supplementary data
Albin Kuriakose: Writing – review & editing, Validation, Software,
Schematic of experimental setup; laser average power calibration
Methodology, Investigation. Pariksha Malik: Writing – review &
plot; optical microscope images of optimisation of laser texturing on

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