Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles
A new modification of nanosphere lithography has been realized to obtain multilayered systems of ordered gold nanoparticles (NP). NP have been formed using vacuum deposition of a 5…60-nm layer of gold on ionic etched multilayered regular coating consisting of several layers of 200-nm polystyrene sph...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2017
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| Cite this: | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles / V.I. Styopkin, V. Liakhovetskyi, V. Rudenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 2. — С. 240-245. — Бібліогр.: 15 назв. — англ. |
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| author | Styopkin, V.I. Liakhovetskyi, V. Rudenko, V. |
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| citation_txt | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles / V.I. Styopkin, V. Liakhovetskyi, V. Rudenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 2. — С. 240-245. — Бібліогр.: 15 назв. — англ. |
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| description | A new modification of nanosphere lithography has been realized to obtain multilayered systems of ordered gold nanoparticles (NP). NP have been formed using vacuum deposition of a 5…60-nm layer of gold on ionic etched multilayered regular coating consisting of several layers of 200-nm polystyrene spheres. Optical study shows that the spectra of NP depend on their thickness and may be changed by heat treatment. Increasing the NP thickness within the 5…20-nm range leads to a shortwave displacement of the plasmon resonance peak position, while the longwave shift is observed in the 20…60-nm range. Heat treatment of NP brings narrowing and displacement of spectral bands, raising the extinction. It has been supposed that variation of the NP shape is the most substantial factor for changes of optical properties in the 5…20 nm thickness region, while electromagnetic coupling between NP in different layers becomes more important for thicknesses larger than 40 nm. Optical properties inherent to the obtained system of NP can be tuned by changing the polystyrene spheres diameter, extent of etching, thickness of gold layer, and with the heat treatment. It may be used in the design of nanophotonic devices.
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Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
240
PACS 78.67.-n
Using nanosphere lithography for fabrication
of a multilayered system of ordered gold nanoparticles
V.I. Styopkin, V.R. Liakhovetskyi, V.I. Rudenko
Institute of Physics, NAS of Ukraine,
46, prospect Nauky, 03680 Kyiv, Ukraine,
E-mail: vis49@mail.ru; lyakh@iop.kiev.ua; val@iop.kiev.ua
Abstract. New modification of nanosphere lithography has been realized to obtain
multilayered systems of ordered gold nanoparticles (NP). NP have been formed using
vacuum deposition of 5…60-nm layer of gold on ionic etched multilayered regular
coating consisted of several layers of 200-nm polystyrene spheres. Optical study shows
that spectra of NP depend on their thickness and may be changed by heat treatment.
Increasing the NP thickness within the 5…20-nm range leads to a shortwave
displacement of the plasmon resonance peak position, while the longwave shift is
observed in 20…60-nm range. Heat treatment of NP brings narrowing and displacement
of spectral bands, rising the extinction. It has been supposed that variation of the NP
shape is the most substantial factor for changes of optical properties in the 5…20 nm
thickness region, while electromagnetic coupling between NP in different layers becomes
more important for thicknesses larger than 40 nm. Optical properties inherent to the
obtained system of NP can be tuned by changing the polystyrene spheres diameter, extent
of etching, thickness of gold layer and with the heat treatment. It may be used in design
of nanophotonic devices.
Keywords: nanosphere lithography, gold nanoparticles, optical properties, heat
treatment, ionic etching.
Manuscript received 03.02.17; revised version received 12.04.17; accepted for
publication 14.06.17; published online 18.07.17.
1. Introduction
Ordered noble metal nanoparticles (NP) are promising
materials for photonic materials, SERS, near-field
optics, etc. Different lithographic techniques are used to
fabricate these nanostructures. The high resolution of NP
production can be obtained with electron beam and
focused ion beam lithography. However, these methods
are serial and expensive, which confines high volume
manufacture of NP. An alternative method for
production of ordered NP with determined shape is the
nanosphere lithography (NSL) [1-3]. NSL is a powerful
process to produce various arrays of periodic structures
that may be used in the field of nano- and
microfabrication. It may be applied in devices of
nanophotonics, such as surface enhanced Raman
scattering substrates, biosensors, design of ordered
nanostructures for ultrahigh density magnetic recording.
In a simplest version, NSL is a two-step process.
The one-layer coating of ordered polystyrene spheres
(PS) is formed on the substrate. Then, a desired material
is deposited on this substrate through holes in the PS
layer. In this way, after PS removal one obtains system
of ordered NP of this material. But coverage of the
substrate with NP is low and amounts 7.2% [4].
NP in the form of metal film on surface of PS may
be used to increase volume of obtained nanostructures
[5, 6]. But the closeness of these NP to each other
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
241
influences strongly on their properties. Moreover, the
size of NP is limited by the used sort of PS.
To overcome these disadvantages, in this work
NSL method was used to produce ordered NP on the
surfaces of etched PS in multilayer coating. Ion etching
the PS in coating allows controlling their size and
distances between them [7, 8]. Besides, in the case of
multilayered coating etching PS in the top layer opens
those in lower layers and increase a number of the
obtained NP. Deposition of metal on the surface of
etched PS creates a complex structure of ordered NP that
are located in different layers. The aim of the work was
to obtain nanostructures, consisted of NP formed on the
surface of etched PS in multilayered coatings, and to
study there optical properties.
2. Experiment
200-nm PS (standard deviation 6 nm) were used to
fabricate the multilayered coatings. PS were supplied by
Sigma-Aldrich (2% aqueous suspension). The coatings
were obtained on glass substrates. Before PS deposition,
the substrates were cleaned and hydrophilized. They
were maintained in Piranha solution (3:1 H2SO4:H2O2) at
70 °C for 1 hour. Then, the substrates were rinsed in
fresh distilled water and sonicated for 30 min in 5:1:1
H2O:NH4OH:H2O2 solution. Before PS deposition, the
substrates were rinsed again in fresh distilled water.
Diluted with distilled water to 0.1% content PS
suspension was drop-coated onto substrate and dried at
35 °C. The volume of deposited PS suspension was
adjusted to obtain coatings with the thickness of three
layers of PS on the substrate. After drying, the coating
was formed on the substrate, the main part of which
contains three and more layers of PS. Lesser part of
substrate was covered with one and two layers of PS.
The PS coatings were etched in JFC-1100 Ion
Sputtering Device (JEOL) under the air pressure close to
0.2 Torr. A degree of PS etching depends on the applied
anode-cathode voltage, air pressure in the chamber,
duration of process, using of ion stream concentrator,
etc. The process conditions were adjusted to obtain PS
diameters 130…150 nm in the upper layer of coating.
Etched PS were covered with gold by using thermal
evaporation in vacuum. The weight thickness of gold
layer varied from 5 up to 60 nm. Thus, it was obtained a
multilayered system of gold NP on the surface of etched
PS. To enhance stability, the NP were thermally treated.
5-min heat treatment was done in air at 270…300 °C. It
should be noted that uncovered PS soften at 120...140 °C
for 5 min, but the gold coating makes it possible to
sufficiently rise the temperature of heat treatment.
Morphology of this multilayer system of gold NP
was studied using JSM-35 scanning electron microscope
(SEM).
Optical spectra of the NP system were obtained
with MDR-6 spectrometer within the range 400 to
800 nm with a non-polarized incident light beam at room
temperature.
3. Results
SEM image of a part of the multilayered PS coating is
shown in Fig. 1a. Two PS are lacking in the upper layer
and PS of the second layer become visible at these
places. Scheme of PS packing in such a coating is shown
in Fig. 1b.
After ion etching, PS in upper layers reduce and PS
of the second and third layers appear. SEM image of the
multilayered PS coating after ion etching and deposition
of the gold layer are shown in Fig. 2a. PS in the upper
layer decrease down to 140…150 nm, while the size of
visible part of PS in the second layer reduces down to
160…170 nm. The scheme of PS packing after etching is
shown in Fig. 2b.
Heat treatment reduces the size of PS and NP on
the PS, correspondingly. The PS and NP sizes reduction
can be observed on SEM image of the system after heat
treatment (Fig. 3). This reduction will give an increase
of NP thickness.
a
b
Fig. 1. SEM image of the multilayered PS coating with defects
in the upper layer (a) and the scheme of this coating (b).
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
242
a
b
Fig. 2. SEM image of the multilayered PS coating after ion
etching : 1 – PS in the upper layer, 2 – PS in the second layer,
3 – PS in the third layer (a); scheme of PS packing after
etching (b).
Fig. 3. SEM image of the multilayered NP system after heat
treatment.
Optical density spectra of the multilayered system
of etched PS after deposition of gold layer of different
thickness and the spectrum of the initial PS coating are
shown in Fig. 4a. The spectra of gold NP on etched PS
reveal broad peaks. The extinction rises with the
increasing of gold layer thickness. The position of
spectra maximum displaces to the lower wavelengths
with thickening the gold layer up to 40 nm. But the
resonance peak of 60-nm NP shifts to a longer
wavelengths in comparison with that of 40-nm NP.
Fig. 4b shows that heat treatment of NP leads to
narrowing the spectral bands, rising the extinction and
displacing the peak position. The value and sign of this
displacement depends on the gold layer thickness. As a
result, the wavelength of spectra maximum lowers with
thickening the gold layer within the range 5…20 nm,
while within the range 20…60 nm of gold thickness the
wavelength rises. Thus, heat treatment gives a different
sign of displacement for the spectra in different regions
of gold NP thicknesses.
a
b
Fig. 4. Optical density spectra of PS coating and of
multilayered system of gold NP with different thicknesses on
the etched PS before (a) and after heat treatment (b).
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
243
Fig. 5 shows the optical density spectra of multi-
layered system of gold NP with the thickness values 20
and 40 nm before and after heat treatment. In the case of
20 nm, the thickness position of spectrum maximum
changes from 604 to 570 nm after heat treatment, while
for the thickness 40 nm – from 557 to 579 nm.
4. Discussion
Optical spectra of noble metal NP are mainly controlled
by localized surface plasmon resonance (LSPR).
Characteristics of this resonance depend on the size,
shape, properties of substrate. They may also be
influenced by electromagnetic coupling between the
adjacent NP. In this work, optical properties of the
multilayered NP system show good correlation with data
of gold NP in other works. The spectra of rectangular
gold NP are calculated in [9]. Peak of dipole LSPR is
obtained at 545 nm for the system of NP with 200-nm
size, 50-nm thickness and interparticle distance of
200 nm. In our work, NP with 150-nm size and 60-nm
thickness show the peak at 575 nm. This 30-nm
displacement may be caused by difference in the NP
shape and influence of substrate.
a
b
Fig. 5. Optical density spectra of the multilayered system of
gold NP on the etched PS before and after heat treatment with
the thickness of gold 20 nm (a) and 40 nm (b).
The conditions of NP formation in [10] are similar
to those of this work. The gold NP with the thickness
30 nm were obtained on 170-nm PS on a glass substrate.
Resulting NP system shows spectra with the peak at
600 nm. This is also close to the results of our work.
To explain changes in the spectra with variation of
NP thickness and after heat treatment, only dipole
resonance has been considered in this work. We
supposed that optical properties of multilayered NP
system mainly depend on the NP thickness and
interaction of electromagnetic fields of nearest NP.
In the region of small NP thickness, its variation
will not change the interparticle distance of the NP in the
same layer. NP of the different layers are placed at quite
large distance, and electromagnetic coupling of NP is
low. Thus, variation of distance between these NP will
not influence sufficiently on their properties, and optical
spectra of NP system mainly depend on variation of
single NP properties.
Thickening the NP will change their shape. This
effect was considered for NP with the shape of spheroids
[11] and rods [12]. Such changing is also studied for
variation of aspect ratio of rectangular gold NP [9].
Calculations show a long wave shift of peak position for
length increase of long side of NP. This displacement is
explained by the influence of phase retardation of
incident radiation and by electrodynamics boundary
effects related with the particle shape. The effect of
phase retardation is revealed at relatively large sizes of
NP, when the induced polarization is not all in-phase for
plane-wave excitation due to the finite wavelength. In
our case, NP sizes are about 150 nm, and effect of phase
retardation may be observed. But the increase in the NP
thickness does not change the NP size in the plane of
incident light polarization, and phase retardation cannot
cause evident changes in the optical spectra. To a greater
extent, it should influence variation of the NP aspect
ratio. Thickening the NP increases the ratio of thickness
to a size of NP that is in the plane of incident light
polarization. Thus, the resonant peak position will shift
to the short wave side.
A similar shortwave shift with NP thickening was
obtained for resonance in Ag nanodisks [12], where it
was shown that such a shift is more significant at a small
thickness.
On the other hand, electromagnetic coupling
between NP will exhibit sufficient effect at larger NP
thickness. This interaction between particle fields
involves both very short-distance interactions due to
evanescent fields and long-range interactions, mainly
due to propagating dipolar fields. It also causes
displacement of the resonant peak. The value and sign of
this displacement depend on orientation of light
polarization relative to interacting NP. Study of
electromagnetic coupling of gold NP pairs [13] shows
that the decrease in distance between NP leads to a
longwave shift of resonance in the case of parallel
orientation of light polarization to the long axis of
particle pairs. In the case of orthogonal orientation of
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
244
light polarization, the shortwave displacement is
observed.
In the considered multilayered system, NP are
located in different layers at various distances. So,
electromagnetic coupling between NP is very
complicated. The scheme of NP arrangement in different
layers is shown in Fig. 6 (side view). The schematic
charge distribution in NP is also given for the excitation
with light having polarization parallel to axis passing the
centers of 1 and 2 NP.
Increasing the NP thickness does not change the
distance between NP 1 and 2 located in one layer.
Distance between NP 3 in the second layer and NP 1 and
2 in upper layer decreases. Thus, thickening the NP will
influence mainly on the electromagnetic coupling
between NP in different layers.
Fig. 7 shows the scheme of NP arrangement in
different layers (top view) and for charge distribution in
them under two orientations of light polarization. In the
case of light polarization in Fig. 7a, electromagnetic
coupling of NP 3 and 4 gives a longwave shift of
resonance. Charges in NP 1 and 2 are arranged almost
symmetrically relative to charges in NP 3 and coupling
between these particles will not change resonance
noticeably. In the case of light polarization in Fig. 7b,
electromagnetic coupling of NP 3 and 4 leads to a
shortwave shift of resonance, while coupling of NP 3
with particles 1 and 2 gives longwave shift. One may
guess that interaction of NP 3 with two particles (1 and
2) gives a larger effect than that with one NP (4). Thus,
it may be supposed that in our multilayered NP system
electromagnetic interaction of NP in different layers will
lead to a longwave shift of resonant peak. But this
interaction will give noticeable effect on plasmonic
resonance only at the small distance between NP.
Results of studying the gold NP [13, 14] show that for
100-nm NP interaction coupling reveals sufficient effect
on optical spectra at the interparticle distance smaller
than 50…60 nm.
Fig. 6. Scheme of arrangement of NP in different layers (side
view) and charge distribution in them under excitation with
light.
Fig. 7. Scheme of arrangement of NP in different layers (top
view) and charge distribution in them under two orientations of
light polarization.
From changes in the PS size after etching, it may
be supposed that the distance between adjacent NP in
different layers amounts about 100 nm. Increasing the
NP thickness up to 30…40 nm will lower the
interparticle distance down to 60…70 nm. Results of
[14, 15] give the longwave shift of resonance 5…10 nm
for these distances.
Therefore, the resonance spectra will reveal a
shortwave shift with the NP thickening mainly due to
variation of single NP properties up to 40 nm thickness.
Subsequent rise of the thickness will increase
electromagnetic coupling of NP at different layers and
lead to a longwave shift of resonance.
The same reasons may explain the changes in
spectra after heat treatment. As it was shown earlier,
heat treatment reduces the size of PS and NP and
increases thickness of NP. The above discussion leads to
a supposition that within the range 0…40 nm the
thickness increasing after heat treatment will shift
resonance to a shortwave part of spectra, while for
thicknesses larger 40 nm – to the longwave part.
5. Conclusions
In this paper, we have shown that using NSL in
combination with the ionic etching allows to obtain
multilayered system of ordered metal NP. Optical
spectra of the initial NP system and thermally treated NP
were studied. It has been shown that optical properties of
the multilayered NP system may be tuned by varying the
NP thickness and heat treatment. Thickening the NP
shifts LSPR spectra, value and sign of displacement
depends on the NP thickness. The heat treatment gives
enlarging the NP thickness and change optical
properties, too. Considering the influence of NP
thickness on spectra has shown two main reasons for
resonance modification. Changing the NP shape is the
most substantial factor in the thickness range 5…20 nm,
while the electromagnetic coupling between NP in
different layers becomes more important for thicknesses
larger than 40 nm.
The proposed system of ordered NP may be used to
design nanophotonic devices.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 2. P. 240-245.
doi: https://doi.org/10.15407/spqeo20.02.240
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
245
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| id | nasplib_isofts_kiev_ua-123456789-214925 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-8034 |
| language | English |
| last_indexed | 2026-03-21T11:50:52Z |
| publishDate | 2017 |
| publisher | Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| record_format | dspace |
| spelling | Styopkin, V.I. Liakhovetskyi, V. Rudenko, V. 2026-03-04T12:49:15Z 2017 Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles / V.I. Styopkin, V. Liakhovetskyi, V. Rudenko // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 2. — С. 240-245. — Бібліогр.: 15 назв. — англ. 1560-8034 PACS: 78.67.-n https://nasplib.isofts.kiev.ua/handle/123456789/214925 https://doi.org/10.15407/spqeo20.02.240 A new modification of nanosphere lithography has been realized to obtain multilayered systems of ordered gold nanoparticles (NP). NP have been formed using vacuum deposition of a 5…60-nm layer of gold on ionic etched multilayered regular coating consisting of several layers of 200-nm polystyrene spheres. Optical study shows that the spectra of NP depend on their thickness and may be changed by heat treatment. Increasing the NP thickness within the 5…20-nm range leads to a shortwave displacement of the plasmon resonance peak position, while the longwave shift is observed in the 20…60-nm range. Heat treatment of NP brings narrowing and displacement of spectral bands, raising the extinction. It has been supposed that variation of the NP shape is the most substantial factor for changes of optical properties in the 5…20 nm thickness region, while electromagnetic coupling between NP in different layers becomes more important for thicknesses larger than 40 nm. Optical properties inherent to the obtained system of NP can be tuned by changing the polystyrene spheres diameter, extent of etching, thickness of gold layer, and with the heat treatment. It may be used in the design of nanophotonic devices. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles Article published earlier |
| spellingShingle | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles Styopkin, V.I. Liakhovetskyi, V. Rudenko, V. |
| title | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| title_full | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| title_fullStr | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| title_full_unstemmed | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| title_short | Using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| title_sort | using nanosphere lithography for fabrication of a multilayered system of ordered gold nanoparticles |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/214925 |
| work_keys_str_mv | AT styopkinvi usingnanospherelithographyforfabricationofamultilayeredsystemoforderedgoldnanoparticles AT liakhovetskyiv usingnanospherelithographyforfabricationofamultilayeredsystemoforderedgoldnanoparticles AT rudenkov usingnanospherelithographyforfabricationofamultilayeredsystemoforderedgoldnanoparticles |