1 s2.0 S0169433221030038 Main
1 s2.0 S0169433221030038 Main
1 s2.0 S0169433221030038 Main
A R T I C L E I N F O A B S T R A C T
Keywords: Theoretical and experimental investigations were performed on the fabrication and polarization property
Wire-grid polarizer enhancement of a single-layer Au grating serving as a wire grid polarizer (WGP) in the mid-wavelength infrared
Extinction ratio (MWIR) range. Femtosecond laser (FSL) annealing was performed to overcome the performance limitations of
Mid-wavelength infrared
the WGP fabricated by nanotransfer printing (NTP), and the results were compared with those of the conven
Hot electron diffused cold-annealing
tional thermal annealing methods using scanning electron microscopy, atomic force microscopy, transmission
electron microscopy, and Fourier transform infrared spectroscopy. Consequently, the extinction ratio of the WGP
annealed with FSL reached up to 1378 (~31 dB) in the 3–5 μm wavelength range, which corresponds to a 2.18-
fold improvement over the non-annealed WGP. This result suggests that it is possible to manufacture MWIR
WGPs at a low cost and over large areas through a simple NTP and FSL annealing process, ultimately yielding
WGPs with improved performances.
* Corresponding authors at: Department of Nano Manufacturing Technology, Korea Institute of Machinery and Materials (KIMM), Daejeon, Republic of Korea.
https://doi.org/10.1016/j.apsusc.2021.151965
Received 12 August 2021; Received in revised form 2 November 2021; Accepted 17 November 2021
Available online 19 November 2021
0169-4332/© 2021 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
H. Kim et al. Applied Surface Science 578 (2022) 151965
etching or lift-off processes increase the manufacturing costs of WGPs. compare the performance of the FSL-annealed WGP. The variation in the
In contrast, the nanotransfer printing (NTP) process has recently transmittance according to the changing nanostructure shape during the
attracted great attention for use in the fabrication of optical devices with annealing process is also studied using the finite-difference time-domain
nanosized metal patterns [12–17]. Thus, NTP can be considered a suit (FDTD) method, and the performance of the manufactured WGP is
able method for the fabrication of metallic subwavelength array struc evaluated.
tures, such as WGPs. During the NTP process, the metallic
subwavelength array patterns can be transferred from a polymer mold to 2. Materials and methods
a rigid and conformal substrate. Owing to the fact that this process does
not require additional etching or lift-off processes, it enables the large- 2.1. Fabrication of the WGP annealed with FSL
area and low-cost production of WGPs.
However, when the Au layer was vertically deposited onto the The NTP process employed for preparation of the WGP is shown in
polymer mold using an evaporator, some amount of Au was deposited Fig. 1a. As indicated, the first step involves the replication of a grating
onto the sidewall of the pattern of the mold. Consequently, when the Au pattern with a width of 200 nm, a period of 400 nm, and a depth of 200
on the mold was transferred to the substrate via the NTP process, the Au nm. Thus, a polymer mold with the above grating pattern was fabricated
present on the line-edge of the pattern was also transferred, resulting in using UV-curable polyurethane-acrylate (PUA) resin 311RM (Minuta
irregular edges on the patterned structures [14,16–18]. Additionally, Technology, Korea). A thermal evaporator system was employed to
the performance of a WGP strongly depends on the shape of the metal deposit Au with a thickness of 150 nm onto the replicated mold (Fig. 1b
wires [19–22], wherein a trapezoidal profile, as opposed to the rectan and 1c). Prior to carrying out the NTP process on the substrate, a 350
gular profile, reduces the ER of the WGP, and this is a common problem nm-thick dielectric spacer composed of benzocyclobutene (BCB) was
during the dry etching and lift-off processes [19–21]. Therefore, the coated on a double-side polished Si wafer. BCB has several advantages,
presence of such irregular metal edges on the optical metal structures including a frequency-independent refractive index (n ≈ 1.54) with a
deteriorate the performances of these structures [14,17]. Furthermore, low loss (k ≈ 10− 4) in the MWIR region (3–5 μm), in addition to
it has been reported that the performances of optical metal nano exhibiting good adhesion to metals and semiconductors, and a low
structures, such as plasmonic structures and WGPs, are degraded by the curing temperature (180–250 ◦ C) [4]. To transfer the Au grating pat
presence of grain boundaries and an increase in surface roughness terns of the mold onto the prepared substrate, mr-APS1 (Micro Resist
[23–29]. The metal films deposited via evaporation or sputtering are Technology, Germany), which acts as an adhesive layer, was coated onto
inherently rough owing to the polycrystallinity of the randomly oriented the substrate (≤10 nm thickness). After subsequently heating the sub
grains of different sizes [30–32]. strate at 150 ◦ C for 1 min, the Au grating on the mold was placed on the
Thermal annealing is used to reduce these defects through recrys adhesive layer-coated substrate and roll-pressed with an appropriate
tallization. Previous studies have shown an improvement in the quality pressure. After heating the substrate for a further 5 min, the Au grating
factor, which is defined as the resonance wavelength divided by the was transferred to the Si substrate, as shown in Fig. 1d and 1e to give the
bandwidth of the resonance peak, of the metallic nanostructures by desired WGP. Finally, annealing was carried out using an FSL with a
increasing the grain size and reducing the surface roughness via thermal laser wavelength of 1030 nm, a laser energy of 0.26 μJ, a beam scanning
annealing. However, the excessive energy required during the thermal speed of 20.0 mm/s, and a laser pulse repetition rate of 100 kHz over 20
annealing process changed the shapes of the metallic nanostructures scans. For comparison, samples of a non-annealed (NA) WGP and a rapid
[26,27]. To address this issue, encapsulation of the metallic nano thermal process (RTP)-annealed WGP treated for 5 min at 150 ◦ C were
structures was examined, and although this prevented deformation of also prepared simultaneously.
the metallic nanostructures during thermal annealing, an additional
deposition process was required [28,29].
In contrast, femtosecond laser (FSL) annealing is a practical method 2.2. Measurement method
for achieving grain growth without deformation of the nanostructure
shape. When metallic nanostructures are irradiated with an FSL, all The morphology change of the WGP was observed using a a scanning
electrons in the electron diffusion length (le ) are excited by the intense electron microscope (SEM, Sirion, FEI, USA) and the surface roughness
laser beam [33,34], and the hot carriers produced by the excited elec of the WGP was investigated using a an atomic force microscopy (AFM,
trons are transported to the interior of the metal. In the context of Au as a XE-100, Parksystems, South Korea). The transmission spectra of WGPs
novel metal for this process, Au is representative of weak electro for the normally incident TE and TM polarizations were measured in the
n–phonon coupling (γAu ) (γAu ≈ 2.3 × 1016 W/m3K) [35]. As the elec wavelength range of 3–5 μm using a Fourier transform infrared (FTIR)
tron–phonon coupling (γ) directly affects the behavior of electrons and spectrometer (NICOLET iS20, Thermo Fisher Scientific, USA). The FTIR
the lattice temperature [33], a low coupling efficiency requires a greater beam was linearly polarized along either the TE or TM direction using a
length of time for thermal equilibrium to be reached. Metallic nano commercial wire grid polarizer (Edmund optics, USA), and the FTIR-
structures with a thickness similar to the le and exhibiting a weak measured transmission spectra were recorded using a deuterated tri
electron–phonon coupling are heated almost homogeneously [34]. The glycine sulfate (DTGS) detector.
transferred heat then increases the internal temperature and grain size.
As a result, FSL annealing can be applied to heat-sensitive nano 3. Results and discussion
structures because the temperature of the entire metallic pattern rises
almost simultaneously and then rapidly decreases through heat transfer When a FSL irradiates a nanostructured metal to induce thermal
by the hot carrier. This avoids the issues related to shape deformation distribution, the key factors are the electron diffusion length and the
that are encountered for other thermal annealing methods. electron–phonon coupling [33,34]. More specifically, the electron
In this study, we report the fabrication of a WGP consisting of a Au diffusion length refers to the depth at which an electron can be excited
√̅̅̅̅̅̅̅̅̅̅̅
grating with a wire width of 200 nm, a period of 400 nm, and a thickness when the FSL is irradiated [34], and is defined as le ≈ 2De τl , where De
of 150 nm using the NTP process. The Au grating of the fabricated WGP and τl are the thermal diffusivity and laser pulse duration, respectively.
possesses many grain boundaries and irregular edges, which limits the The approximate value of le obtained through the thermal diffusivity of
performance of the WGP. Thus, to overcome the performance limitations Au and the pulse duration of our FSL source was 130 nm. In addition, the
of the WGP, post-annealing processing is performed using the FSL electron–phonon coupling determines the cooling of the electron bath
method. Additionally, rapid thermal processing (RTP) is carried out to and the time required to reach thermal equilibrium. The difference in
the electron–phonon coupling indicates the temperature gradient that
2
H. Kim et al. Applied Surface Science 578 (2022) 151965
Fig. 1. (a) Schematic of the WGP manufacturing process based on NTP and FSL annealing. (b) Photographic image and (c) focused ion beam (FIB) image of Au
deposited on a replica mold. (d) Photographic image and (e) Scanning electron microscopy image of a WGP transferred by the NTP process on a Si substrate.
3
H. Kim et al. Applied Surface Science 578 (2022) 151965
Fig. 2. (a) Temporal profiles of Te and Ti along the two interfaces, and (b) distribution of the lattice temperature after the absorption of a 350 fs laser pulse as a
function of thickness and time in the gold/silicon structure.
Fig. 3. SEM images of (a) a non-annealed (NA) WGP, (b) an RTP-annealed WGP, and (c) an FSL-annealed WGP. (d)–(f) AFM images of the surfaces of the WGPs
fabricated using the NTP process: (d) the non-annealed WGP, (e) the RTP-annealed WGP, and (f) the FSL-annealed WGP.
unchanged, as shown in Fig. 3c, and the roughness values of the edges
and surfaces were reduced. Table 2
Surface roughness data for each sample, as obtained by AFM measurements.
For a more detailed analysis of the surface of each WGP, AFM images
were obtained in non-contact mode, as shown in Fig. 3d–f. In addition, NA RTP FSL
as indicated in Table 2, the surfaces of the RTP-annealed and the FSL- Ra (Roughness average, nm) 6.592 6.265 4.453
annealed WGPs exhibited reduced surface roughnesses compared to Rq (RMS roughness, nm) 8.246 7.561 5.591
that of the non-annealed WGP. More specifically, the surface roughness
averages (Ra ) of the non-annealed WGP, RTP-annealed WGP, and FSL-
annealed WGP were determined to be 6.592, 6.265, and 4.453,
respectively, while the root-mean-square of the surface roughness (Rq )
4
H. Kim et al. Applied Surface Science 578 (2022) 151965
values of the non-annealed WGP, RTP-annealed WGP, and FSL-annealed from the Au grating to reduce the surface roughness and enlarge the
WGP were 8.246, 7.561, and 5.591, respectively, which shows a similar grain size, the ER of the RTP-annealed WGP was degraded owing to the
trend to that of Ra . Consequently, the surface roughness was reduced for shape change of the Au grating (i.e., from an elliptical to a rectangular
the RTP- and FSL-annealed WGPs compared to the non-annealed WGP. profile). In addition, the width of the Au grating increased, while the
In particular, in the case of the FSL-annealed WGP, the values of Ra and thickness decreased. In this context, it should be noted that the TM
Rq decreased by a factor of ~1.5 compared to the non-annealed WGP. transmittance of a WGP decreases as the width of the Au grating at a
This significant reduction in the surface roughness for the FSL- fixed period increases, whereas the TE transmittance of a WGP increases
annealed WGP is also shown in Fig. 4. More specifically, Fig. 4a–c as the thickness of the Au grating decreases [21,44].
show TEM cross-sectional images of the non-annealed, RTP-annealed, To understand the influence of the surface roughness, grain size and
and FSL-annealed WGPs, respectively, wherein it is apparent that the shape of the Au grating on the performance of the WGP, FDTD simula
surface roughness of the FSL-annealed WGP was lower than that of the tions were performed using commercial software (Lumerical FDTD So
non-annealed WGP. Furthermore, the grain size of the FSL-annealed lution). The permittivity of Au in MWIR was described by the Drude
WGP increased compared to that of the non-annealed WGP. model with a plasma frequency ωp = 1.378 × 1016 rad/s and a damping
The polycrystallinity of the Au nanostructure prior to annealing is constant Γ = 4.08 × 1013 rad/s. The increase in the optical loss due to the
shown in the TEM image of Fig. 4a, where small grains can be observed, surface roughness and grain boundary effects can be described by
while the annealed WGPs, as shown in Fig. 4b and c, exhibit fewer grain increasing the damping constant of the Drude model. Fig. 5d and 5e
boundaries and larger grains. This can be accounted for by considering show the simulated transmission spectra of the TM and TE modes of the
that the RTP and FSL annealing processes provide heat energy to the WGP for damping constants of 1, 3, and 5 times that of Au. As the
grain of the Au nanostructure. More specifically, when thermal energy is damping constant of the Au increased, the TM transmittance decreased
applied to the grain, recovery occurs, in which the residual stress is slightly and the TE transmittance slightly increased, resulting in a slight
released. Around the end of the recovery period, recrystallization be reduction in the ER, as shown in Fig. 5f. To confirm the elliptical profile
gins, and the grain size increases. Although the melting point of Au is effect of the Au grating, the simulated transmission spectra for the TM
known to be 1064 ◦ C, recrystallization generally occurs at a temperature and TE modes of the WGP for the Au grating with rounded corners with
of approximately 1/3 to 1/2 of the absolute melting point of the material different radii (r) were obtained (Fig. 5h and 5i). As the radius of the
in Kelvin. Thus, both the RTP and FSL annealing methods provide suf rounded corners of the Au grating increased, the TM transmittance
ficient thermal energy for recrystallization and grain growth [39,40]. decreased and the TE transmittance increased significantly, resulting in
Fig. 5a and b show the measured transmission spectra for the TM and a severe reduction in the ER, as shown in Fig. 5j. Thus, the degradation
TE modes of the non-annealed, RTP-annealed, and FSL-annealed WGPs. in the performance of the RTP-annealed WGP was mainly caused by the
The performance of the WGP as a polarizing filter can be evaluated by deformation in the shape of the Au grating. Our results therefore suggest
measuring the ER (TTM /TTE ), as shown in Fig. 5c. As indicated, the TM that the FSL annealing method can also contribute to improving the
transmittance of the FSL-annealed WGP increased by >90% at a wave optical performances of plasmonic nanostructures and metamaterials by
length of 3.4 μm, and remained >85% over the wavelength range of 3–5 reducing the optical damping.
μm. In contrast, the TE transmittance of the FSL-annealed WGP
decreased in the wavelength range of 3–5 μm compared with that of the 4. Conclusions
non-annealed WGP. Overall, the FSL-annealed WGP showed the highest
TM transmittance and the lowest TE transmittance, which resulted in the In this study, a high-performance mid-wavelength infrared (MWIR)
highest ER. The highest ER values obtained for the non-annealed WGP, wire grid polarizer (WGP) was fabricated using femtosecond laser (FSL)
RTP-annealed WGP, and FSL-annealed WGP were 631, 202, and 1378 annealing. FSL annealing induces two phenomena; initially, the grains of
(~31 dB), respectively, whereas the average ER values exceeded 470, the Au nanostructures grow owing to the hot carrier effect, wherein the
140, and 820, respectively, in the wavelength range of 3–5 μm. These hot carriers simultaneously increase the temperature of the entire
results indicate that the FSL-annealed WGP exhibited an excellent per metallic pattern prior to rapidly reducing the temperature. Therefore,
formance compared with earlier WGPs fabricated using complex pro FSL annealing allows grain growth to occur without any deformation in
cesses or structures [4,41–43]. As expected, FSL annealing, which the nanostructure shape. In terms of the second phenomenon, FSL
removed the irregular metal edges from the Au grating, reduced the annealing imparts a polishing effect on the non-planar surface because
surface roughness of the Au grating, and enlarged the grain size of the heat transport is more efficient when a femtosecond laser beam is irra
grating without any shape deformation, thereby enhancing the perfor diated on the irregular metal edges of the Au wires introduced by a
mance of the WGP. The highest ER of the FSL-annealed WGP increased transfer process. Based on these factors, the performance of the FSL-
by a factor of ~2.18 compared with that of the non-annealed WGP. annealed WGP was approximately 2.18 times higher than that of the
However, although RTP annealing removed the irregular metal edges non-annealed WGP, and its extinction ratio reached 1378 (~31 dB).
Fig. 4. TEM cross-sectional images of the surfaces of (a) the non-annealed, (b) the RTP-annealed, and (c) the FSL-annealed WGP.
5
H. Kim et al. Applied Surface Science 578 (2022) 151965
Fig. 5. Measured transmission spectra of the (a) TM and (b) TE modes, and (c) the extinction ratio for the non-annealed, RTP-annealed, and FSL-annealed WGPs.
Simulated transmission spectra of the (d) TM and (e) TE modes, and (f) the extinction ratio for the WGPs based on the damping constant of the Au layer. Simulated
transmission spectra of the (h) TM and (i) TE modes, and (j) the extinction ratio for the WGPs based on the radii (r) of the rounded corners.
However, the WGP annealed using the conventional rapid thermal Declaration of Competing Interest
processing method exhibited a poorer performance than the non-
annealed WGP owing to deformation in the shape of the Au grating, The authors declare that they have no known competing financial
as verified through finite-difference time-domain simulations. In interests or personal relationships that could have appeared to influence
conclusion, MWIR WGPs fabricated via NTP and annealed using an FSL the work reported in this paper.
exhibit an improved selectivity and lack of substrate damage, thereby
shortening the process time, and increasing productivity. Therefore, this Acknowledgement
materials could be applied in the areas of optical nanostructures, plas
monic nanostructures, metamaterials, and high-performance polariza This work was supported by the National Research Foundation of
tion imaging systems that require miniaturization and on-chip Korea (NRF) funded by the Ministry of Science and ICT
integration. (2018M3A7B4069995, 2020M3D1A2101787, 2014M3A6B3063707,
2014M3A6B3063700) and the Basic Research Fund of the Korea Insti
tute of Machinery and Materials (NK230E).
CRediT authorship contribution statement
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