Surface plasmon resonance and coloration in stainless steel with a 2D periodic texture

Applied Physics A
(2019) 125:624
https://doi.org/10.1007/s00339-019-2926-9
Surface plasmon resonance and coloration in stainless steel with a 2D
periodic texture
Minseok Seo1 · Myeongkyu Lee1
Received: 10 March 2019 / Accepted: 9 August 2019
© Springer-Verlag GmbH Germany, part of Springer Nature 2019
Abstract
Although stainless steel (STS) is an alloy commonly used in both daily life and the industrial field, little is known about its
plasmonic behavior. In this study, we investigated the surface plasmon resonance (SPR) phenomenon in two-dimensionally
(2D) textured STS. A 2D periodic grating with a 500 nm pitch was fabricated by imprinting combined with electrochemical etching on the surface of 316L STS plates. Since the fabricated surface texture gave rise to SPR absorption peaks and
structural colors, its resonance behavior was characterized in terms of light incident direction and polarization state; the
dependence of the SPR wavelengths on these two parameters was theoretically calculated based on the grating-assisted lightcoupling mechanism. The experimental results were in good agreement with the theoretical calculations. Grating-coupled
SPR can be an effective tool to generate structural colors in STS and may be used in many applications including surface
decoration, product identification, and anti-counterfeiting.
1 Introduction
The widespread use of metals in vehicles, electronic devices,
machines, and tools is attributed to their superior mechanical
and electrical properties. Although the mechanical performances of metals are still of primary interest, their optical properties have also drawn increasing attention [1–6].
With the rapidly growing application of metals for mobile
electronics, home appliances, and building interiors, their
esthetics becomes increasingly significant; surface decoration with sensuous colors is an essential feature to improve
the appearance of materials. Over the past decade, metal
plasmonics has received great attention due to its promising
applicability in many different areas, including solar cells
[7, 8], displays [9, 10], sensors [11], color filters [12], art/
decoration, and anti-counterfeiting [13]. It benefits from the
coupling of light with charges such as electrons in metals.
Surface plasmons are charge oscillations propagating along a
metal–dielectric interface. Surface plasmon resonance (SPR)
is the resonant oscillation of free electrons excited by incident light, which is coupled into a metal–dielectric interface
to generate the oscillation. Thus far, SPR studies have been
* Myeongkyu Lee
[email protected]
1
Department of Materials Science and Engineering, Yonsei
University, Seoul 120‑749, South Korea
carried out mostly with precious metals like gold and silver,
which are both known as good plasmonic materials.
Stainless steel (STS) is one of the most widely used metals in daily life. Several different methods have been investigated to color or decorate the surface of STS, including
direct current anodization [14], surface passivation with
an oxide layer [15–17], and laser-direct surface structuring [18–22]. However, they all present some drawbacks:
although anodic films can produce different colors depending on the anodization conditions, they are easily cracked on
drying; forming a passivation layer with uniform thickness
and coloration on an STS surface is still challenging; and the
surface structures obtained by laser processes are only statistically reproducible. In contrast, SPR provides an effective
way to manipulate the absorption and reflectance of light
in a specific wavelength range, producing structural colors.
We have recently demonstrated SPR on bulk STS having a
one-dimensional (1D) surface texture [23], but it was supported only when the incident light had a polarization parallel to the grating vector, showing colors under this transverse
magnetic (TM) polarization. In this study, we investigated
SPR in STS with a two-dimensional (2D) periodic texture,
aiming to produce colors under both transverse electric (TE)
and TM polarizations. A 2D texture with a 500 nm pitch
was fabricated by imprinting and electrochemical etching
on the surface of STS plates. The resonance behavior of the
surface texture and the obtained colors were characterized
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M. Seo, M. Lee
in terms of light incident angle and polarization. The SPR
positions were theoretically calculated using the measured
dielectric function of the STS alloy tested, and they were
compared with the experimental results. This study may
provide a design rule for producing SPR-based structural
colors in STS.
2 Materials and methods
The samples used for this study were prepared from commercial 316L STS plates (thickness = 1 mm, super mirror
polished), which were cut into 20 mm × 20 mm pieces. The
refractive index, N = n + ik, of 316L STS was measured as a
function of the photon energy by ellipsometry using a polished sample. The dielectric function ε of the sample was
derived from the relation of ε = εm + iεm′ = N2 = (n + ik)2,
where εm and εm′ are the real and imaginary dielectric constants, respectively. εm depends on both the real and imaginary refractive indices as εm = n2 − k2; the measured refractive indices are plotted in Fig. 1 along with the derived εm.
The central areas (~ 10 mm × 10 mm each) of the samples
were textured by imprinting combined with etching. Figure 2
shows a schematic illustration of the fabrication process.
An SU-8 photoresist (PR) layer was deposited onto the STS
surface by spin coating and successively imprinted using a
polyurethane acrylate (PUA) mold, which was cast from a Si
master stamp having a 2D square-lattice pattern fabricated
by photolithography and wet etching of a (100)-oriented Si
wafer. The pattern pitch was 500 nm, which is the minimum scale obtainable with conventional photolithography.
The imprinted PR layer was cured by ultraviolet (UV) light,
Fig. 1 Measured refractive indices and derived real dielectric constant
13
Fig. 2 Schematic of the texture patterning process of stainless steel
(STS) plates
baked at 150 °C, and then partially removed via reactive ion
etching (RIE) so that the STS surface was locally exposed.
Then, the exposed STS surface was etched using two different methods: acid etching, with an HCl solution, and electrochemical etching. The latter was performed according to the
method described in a literature report [24]; the sample and
a Cu block were immersed in an aqueous solution of oxalic
acid and, respectively, used as anode and cathode. Finally,
the residual PR layer was removed using a piranha solution.
The microstructural analysis of PUA mold, PR layer, and
final texture was performed using a field-emission scanning
electron microscope (SEM) (JSM-7001F, JEOL Inc. 15 kV).
The texture heights were measured with an atomic force
microscope (AFM). Reflectance spectra were measured by
a UV–visible spectrophotometer using a halogen lamp as the
light source. The polarization of light was controlled by a
linear polarizer. The incident angle of light was varied from
10° to 30° with respect to the normal to the sample surface.
The camera images of the samples were taken using a digital
camera. A sheet polarizer was placed between the camera
and the sample. Full-wave electromagnetic simulation was
performed using finite-difference time-domain (FDTD) simulation software (www.lumeri​ cal.com). A plane-wave source
in the wavelength range from 300 to 800 nm was incident
onto the sample surface. The incident angle of light was varied from 0° to 40°. The spectral reflectance was measured by
a power monitor placed above the sample. The electric- and
Surface plasmon resonance and coloration in stainless steel with a 2D periodic texture
magnetic field distributions were obtained by placing a field
profile monitor at the cross-section of the sample.
3 Results and discussion
3.1 Fabrication of textured STS surface
Figure 3 shows a 2D texture formed on the surface of STS,
together with its fabrication steps. Since the Si stamp used
had inverse pyramidal trenches, the PUA mold cast from
it exhibited sharp tips. However, these mold tips could not
reach the top surface of the STS samples by imprinting
alone, even with the application of a high pressure. This
is the reason for employing the intermediate RIE step to
expose the STS surface. The width of the texture grooves
was also affected by the RIE time, although it depended
predominantly on the STS etching time. The final texture
morphology was influenced by many experiment factors.
First of all, to produce texture patterns of high quality and
uniformity, the PUA mold should be a perfect replica of the
Si stamp; to this end, the PUA solution must uniformly coat
the stamp. On the contrary, when the features formed on
the PUA mold have nonuniform heights, the resulting STS
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624
texture is irregular, as shown in Fig. 4a. For the imprinting,
the PUA mold was placed on top of the PR-coated sample
and pressed with a mechanical press. However, this direct
pressing often broke the mold. This problem was solved by
inserting a polydimethylsiloxane (PDMS) plate between the
mold and the press, which was attributed to the higher softness and ductility of PDMS compared to PUA. The exposed
STS surface was first etched with an HCl solution. But the
residual PR layer was easily damaged by this etchant, resulting in holes with irregular shapes (Fig. 4b). On the other
hand, 2D textures with uniform feature sizes were obtained
by electrochemical etching, as shown in Figs. 3 and 4c.
Hence, the sample shown in Fig. 4c was used for the current SPR analysis. The height of the 2D texture, measured
by AFM, was ~ 60 nm.
3.2 Theory of grating‑coupled SPR
For a light wave with wavelength λ travelling in free space,
the relation between its wave vector magnitude Klight (= 2π/λ)
and angular frequency ω is linear: Klight = ω/c, where c is the
light speed in free space. On the contrary, surface plasmons
propagating on a planar metal surface have a nonlinear dispersion relation [25–27]:
Fig. 3 Scanning electron microscope (SEM) images showing
the steps used to fabricate a
two-dimensional texture on a
STS surface
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M. Seo, M. Lee
Fig. 4 SEM images of 2D textures on STS plates obtained using a a PUA mold with nonuniform heights b by typical acid etching with an HCl
solution, and c by electrochemical etching. All scale bars are 1 μm
𝜔
Ksp =
c
√
𝜀m
.
1 + 𝜀m
(1)
Since εm is frequency-dependent and has negative values
in the visible range, the wave vector (i.e., the momentum)
of light is always smaller than that of surface plasmons at a
given ω value (i.e., Klight < Ksp). For SPR to occur, both energy
and momentum should be conserved (i.e., ωlight = ωsp and
Klight = Ksp). A promising way to modify the momentum of
incident light and consequently support SPR is to form a diffraction grating on the metal surface [27–29]. Before discussing SPR based on a 2D grating, we will describe the resonance
condition of a 1D grating. Consider the 1D grating with pitch
d shown in Fig. 5a, where the y-direction is parallel to the grating grooves and the x-direction is parallel to the grating vector
G, whose magnitude is given by G = 2π/d. Suppose that a light
wave with wave vector Ki impinges on the grating at an angle
Fig. 5 a Light diffraction by a
1D grating. b Vector representation of the momentum-matching
condition. c Dispersion relations
of light and surface plasmons
on a planar metal surface. d
Dispersion relations of light
and surface plasmons when a
diffraction grating with pitch d
is present
13
θi with the surface normal in the x–z plane. The incident light
is diffracted into multiple beams according to the following
diffraction relation [30]:
)
(
Ki sin𝜃m − sin𝜃i = mG.
(2)
Here, m represents the diffraction order (m = 0, ± 1, ± 2,..)
and θm is the diffraction angle. The m = ± 1 terms can induce
a strong diffraction effect. The diffracted beams have a wave
vector component tangential to the surface given by Ki sin θm.
If this component equals the wave vector (i.e., the momentum)
of the surface plasmons, both energy and momentum can be
conserved. This condition is mathematically given by
±Ksp = Ki sin𝜃m = Ki sin𝜃i + mG
and alternatively expressed as
±Ksp − mG = Ki sin𝜃i .
(3)
(4)
Surface plasmon resonance and coloration in stainless steel with a 2D periodic texture
The ± sign is added to Ksp because surface plasmons can
propagate either in the positive or negative x-direction. Figure 5b illustrates the relationship between three vectors Kll,
G, and Ksp, where Kll is the component of Ki tangential to
the surface and Ksp is the wave vector of surface plasmons.
Since the magnitude of Kll is Kll = Ki sin θi, the vector form
of Eq. (4) is ± Ksp − mG = Kll. In the absence of a grating (i.e., G = 0), Ksp is always larger than Ki sin θi = (ω/c)
sin θi at the same energy (i.e., at the same ω), because,
as mentioned above, εm has negative values in the visible
range. This is graphically depicted in Fig. 5c, where ω/c is
drawn as a function of the x-component of the momentum
Kx for both light (i.e., Kx = Ki sin θi) and surface plasmons
(i.e., Kx = Ksp). The in-plane momentum (i.e., the tangential
component of the wave vector) of light is modified by a
diffraction grating. This is equivalently viewed as a shift
of the dispersion relation of surface plasmon by mG, as
described in Eq. (4) and illustrated in Fig. 5d. Hence, as
shown, SPR occurs at two different frequencies ω1 and ω2,
which means that, for a given incident angle, two different
light wavelengths λ1 (= 2πc/ω1) and λ2 (= 2πc/ω2) can be
coupled with surface plasmons and, thus, strongly absorbed.
As the incident angle changes, the slope of the “Kx/sin θi”
line also changes, consequently shifting the wavelengths at
which SPR occurs. The SPR wavelengths also depend on
εm and d. The above derivations of Eq. (1) through (3) are
purely based on grating-coupled SPR, where one wave vector is taken from the diffraction theory of a periodic structure
and the other is taken from the surface plasmon theory of a
flat metal surface without periodicity. Today, there exists a
deeper understanding of the nature of resonances on optical gratings. The resonances are explained via the existence
of specific poles of the field function, associated with the
so-called grating modes of periodic open resonators [31,
32]; these grating modes exist even if there is no substrate.
Nevertheless, the simpler grating-coupled SPR mechanism
may also predict fairly correct resonant wavelengths for the
surface texture described in the current study.
Now, we go back to the 2D grating case. A 2D squarelattice texture can be regarded as a superposition of two
orthogonal 1D gratings. Consider the 2D texture shown in
Fig. 6a, where two orthogonal grating vectors are oriented
in the x- and y-directions and have the same magnitude
G = 2π/d. Here, we consider the case where the y–z plane
is the plane of incidence; however, the result using the x–z
plane would be the same due to a rotational symmetry. With
respect to the geometry shown in Fig. 6a, the x-component
of the momentum is
Kx = m1 G
and the y-component is
Ky = Ki sin𝜃i + m2 G,
(5)
(6)
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where m1 and m2 are integers representing the diffraction
order for each grating. Energy and momentum can be simultaneously conserved if Ksp equals the vector summation of
these two components (i.e., Ksp = (Kx2 + Ky2)1/2), leading to
√
(
)
)
(
𝜀m
m1 𝜆 2
m2 𝜆
(7)
−
±
.
sin𝜃i = −
d
1 + 𝜀m
d
Equation (7) can be solved unless m1 and m2 are both
zero.
3.3 Reflection spectra and revealed colors
The reflectance spectra were measured as a function of θi
using the 2D texture shown in Fig. 4c. Figure 6b shows the
experimental spectra obtained under TE-polarized light,
where the electric field of light is parallel to the x-direction. The TE-polarized light exhibited a strong resonance
peak whose position depended on the incident angle. The
resonance peak shifted toward shorter wavelengths as θi
increased. For a 1D grating, SPR does not occur under TE
polarization and thus no color is observed [23]. The TMpolarized light, having the electric field lying in the plane
of incidence, generated two prominent resonance peaks
(Fig. 6c). These two absorption peaks were more widely
separated with an increasing incident angle. The TE-spectra
revealed an additional set of weak peaks in a shorter wavelength range, which were also observed under TM light.
They slightly red-shifted as θi increased. These secondary
peaks overlapped stronger main peaks at some incident
angles, making it difficult to define their positions precisely.
In a 1D grating, the diffraction order m supporting SPR is
either 1 or − 1. According to Eq. (7), however, some different combinations of m1 and m2 are possible in a 2D texture and the curves resulting from its solution are plotted in
Fig. 7. The experiment results agreed fairly well with these
curves. The data corresponding to the curve having m1 = ± 1
and m2 = 1 were not marked due to the absence of any noticeable peaks, which may be because the corresponding resonance peaks were either inherently too weak to be detected
or located outside of the operation range (350–1000 nm)
of the spectrophotometer used. The curve corresponding
to m1 = ± 1 and m2 = 0 was produced by the grating vector
parallel to the x-direction when the incident light was TEpolarized. Since m2 = 0, the grating with the vector parallel
to the y-direction had no contribution to the resonance peaks
of this curve. By the same token, two branches corresponding to m1 = 0 and m2 = ± 1 and the resulting SPR peaks arose
from the grating with the vector parallel to the y-direction. In
this case, the SPR was supported by TM polarization. When
both gratings contribute to the resonance, m1 and m2 are both
non-zero, which produces another set of branches starting
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Fig. 6 a Schematic of light
incidence into a 2D squarelattice texture. Reflectance
spectra obtained from the 2D
texture shown in Fig. 4c under
b TE-polarized light and c TMpolarized light
13
M. Seo, M. Lee
Surface plasmon resonance and coloration in stainless steel with a 2D periodic texture
Fig. 7 Experimental results compared with the theoretical curves predicted by Eq. (7)
at a shorter wavelength (~ 395 nm). The color of an opaque
object is determined by its reflectance spectrum. Using colorimetric transformations, the measured reflectance spectra
were mapped as points on a CIE chromaticity diagram, as
shown in Fig. 8a. Unlike the 1D grating case, the fabricated
2D texture exhibited colors under both polarizations, which
were incident angle-dependent. For comparison, Fig. 8b
shows the camera images of the sample captured apparently
at the same angles. The marked angle represents the angle
between the line connecting the camera to the sample and
the normal to the sample surface. Polarized images were
obtained with a sheet polarizer placed between the camera and the sample. The slight discrepancies observed in
the color appearance may have two reasons; first, while the
spectrophotometer measures the incident angle precisely,
Page 7 of 9
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accurately defining the incident angle when taking camera images is very difficult; second, an object may exhibit
slightly different colors under different light sources, and the
images shown in Fig. 8b were captured under illumination
by a fluorescent lamp in the laboratory. For normal incidence
(i.e., at θi = 0°), the reflectance spectrum and color are the
same for both polarizations. In other words, there is no distinction between TE and TM polarizations. This is obvious
from the curves shown in Fig. 7, although the reflectance
at θi = 0° cannot be measured experimentally. As described
above, the experimental results obtained using the fabricated
2D grating were well predicted by Eq. (7). This implies that
the SPR wavelengths and the revealed colors may be tailored
by varying the grating pitch over a certain range.
Figure 6 shows that the positions of the resonance peaks
depend on the polarization of light. This indicates that the
observed spectra and colors are due to SPR, not diffraction. To confirm this, FDTD simulation was performed for
a 2D texture structure. The pitch, height, and aspect ratio
of the simulated structure were 500 nm, 60 nm, and 0.5,
respectively. Figure 9a shows the reflectance spectra of TMpolarized light simulated at three different incident angles
(θi) of 10°, 20°, and 30°. The peak positions in the simulated
spectra were fairly consistent with the experimental results
(Fig. 6c). Figure 9b shows the magnetic field (H-field) profiles observed at θi = 20°. At λ = 750 nm where no absorption occurs, the field profile appears like a typical reflection
profile. At the peak wavelengths of 685 and 470 nm, the
fields are highly localized and enhanced on the surface of
the grating (i.e., at the air–metal interface), confirming the
excitation of SPR. Since the light is incident at 20° with
respect to the surface normal, the field enhancement is
asymmetric. Figure 9c shows the field profiles observed at
θi = 10°. Compared to the peak for λ = 470 nm and θi = 20°,
the resonance peak found at λ = 460 nm and θi = 10° is wider,
exhibiting a different field-enhancement profile. In Fig. 7,
Fig. 8 a Mapping of the reflectance spectra, obtained under TE and TM polarizations, onto a CIE chromaticity diagram. b Camera images of the
sample. The size of each image is 5 mm × 5 mm
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M. Seo, M. Lee
Fig. 9 a Reflectance spectra of TM-polarized light simulated at three different incident angles (θi) of 10°, 20°, and 30°. b Magnetic field
(H-field) profiles observed at θi = 20°. c Field profiles observed at θi = 10°
two branches (m1 = ± 1 and m2 = − 1, m1 = 0 and m2 = 1)
overlap near θi = 10°. The wider resonance peak and the corresponding field profile may thus result from a combination
of two resonance modes. The theoretical derivations given
in this work are purely based on grating-coupled SPR. For
nanoscale gratings with a pitch much smaller than the wavelength of light, localized SPR (LSPR) may be dominant over
the grating-coupled SPR [13, 28, 33]. In such cases, Eq. (7)
may not be applicable and the overall plasmonic behaviors
should be studied numerically or experimentally because
LSPR with metal nanostructures other than spheres cannot
be described analytically.
4 Conclusion
We theoretically calculated and experimentally demonstrated grating-coupled SPR in 2D-textured stainless steel.
A periodic 2D grating with a 500 nm pitch was fabricated
on the surface of 316L STS plates by imprinting combined
with electrochemical etching and the resulting resonance
behavior was characterized in terms of the incident angle of
13
light and its polarization state. The dependence of the SPR
wavelengths on these two parameters was theoretically calculated based on the grating-assisted light-coupling mechanism. The experimental results were in good agreement
with the calculated ones. Surface texturing and the resulting
resonance absorption present a promising method to produce
structural colors in stainless steel and may find many applications including surface decoration, product identification,
and anti-counterfeiting.
Acknowledgements This work was supported by the R&D convergence program of the National Research Council of Science & Technology of Korea (CAP-16-10-KIMS).
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