delayed freezing of water droplet on silver nanocolumnar film
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8/12/2019 delayed freezing of water droplet on silver nanocolumnar film
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Highly sensitive superhydrophobic Ag nanorods array substrates for surface enhanced
fluorescence studies
Samir Kumar, Pratibha Goel, Dhruv P. Singh, and J. P. Singh
Citation: Applied Physics Letters 104, 023107 (2014); doi: 10.1063/1.4861836
View online: http://dx.doi.org/10.1063/1.4861836
View Table of Contents: http://scitation.aip.org/content/aip/journal/apl/104/2?ver=pdfcov
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Highly sensitive superhydrophobic Ag nanorods array substrates for surfaceenhanced fluorescence studies
Samir Kumar, Pratibha Goel, Dhruv P. Singh, and J. P. Singha)
Department of Physics, Indian Institute of Technology Delhi, Hauz Khas, New Delhi 110016, India
(Received 15 October 2013; accepted 21 December 2013; published online 14 January 2014)
We report a facile method to fabricate highly sensitive superhydrophobic Ag nanorods (AgNR)
arrays based surface enhanced fluorescence spectroscopy (SEFS) substrates using glancing angledeposition technique at a substrate temperature of 133 K and then subsequent coating of
heptadecafluoro-1-decanethiol (HDFT) molecules. The SEFS enhancement behaviour of these
substrates was determined by using aqueous solution of Rhodamine 6G. The HDFT coated
superhydrophobic AgNR arrays SEFS substrates exhibit more then 3-fold fluorescence signal
enhancement than conventional AgNR films. These HDFT coated superhydrophobic AgNR
SEFS substrates based sensors may find application for the purpose of trace analysis and
biosensing. VC 2014 AIP Publishing LLC. [http://dx.doi.org/10.1063/1.4861836]
Superhydrophobic surfaces having contact angle more
than 150 has been a topic of great interest of many research-
ers because of its potential applications in anti-biofouling
paints for boats,1 anti-sticking of snow for antennas,2 self-
cleaning of windshields,3 anti-icing,4 anti-corrosion,5 and in
the field of spectroscopy too.6 Superhydrophobic surfaces
can be fabricated either by chemically modifying the rough
surface with a low surface energy material3 or by creating a
porous or the solidair composite surface by synthesis of
micro- and nanostructures of a hydrophobic material.
Superhydrophobic surfaces have been prepared by many
researchers for various applications using glancing angle
deposition (GLAD) technique.79
GLAD has emerged as a versatile technique to grow
nanostructures ofwiderange of materials with various sizes
and morphologies.
1014
These nanostructures find importantapplications in several fields like gas sensing, optically active
films, photocatalysis, photoniccrystals, and in modifying the
surface wetting properties.1517 Recently, silver nanostruc-
tures grown by GLAD have attracted a significant interest
due to their promising applications in surface plasmon based
studies and for the fabrication of highly sensitive surface
enhanced Raman scattering (SERS) substrates.1820
Surface
enhanced fluorescence (SEF) is another surface plasmon
based phenomenon which has recently emerged as a powerful
technique to improve the fluorescence sensitivity and take the
fluorescence signals with higher contrast level.21,22 SEF is a
giant enhancement of fluorescence intensityof a fluorophore
in the vicinity of a rough metal surface.23,24
Enhancement ofmolecular fluorescence is of great interest due to its immense
application in the field of chemistry, molecular biology, mate-
rials science, photonics and medicine. For the practical appli-
cation of active SEF substrates, one of the key issues is high
enhancement ability and good stability. Till now, various
SEF active substrates have been fabricated ranging from
roughenedsilver electrodes,25 light deposited silver,26 silver
fractals,27 and deposited colloids.28 Another way to fabricate
SEF substrate is by tailoring the surface properties which
may heavily influence the intensity of SEF signal as the giant
enhancement only happen in the close vicinity of the metal
surface. Nanorods arrays were also widely used for the con-
struction of SEF substrates.19,29 Recently, fabrication of
superhydrophobic substrates for enhanced fluorescence using
optical lithography and ion-etching was reported by Gentile
and researchers.30 However, the fabrication method implied
was complex, expensive, and also technologically demanding
for the large scale production.
In this study, we report fabrication of heptadecafluoro-1-
decanethiol (HDFT) coated superhydrophobic Ag-nanorods
substrates for SEF using low temperature GLAD technique.
The HDFT coated superhydrophobic AgNR arrays susbtrates
exhibit more then 3-fold fluorescence signal enhancement
than the conventional AgNR films that may be because ofthe superhydrophobic condensation effect.31,32
Silver nanorod arrays were grown on Si(100) substrates
by thermal evaporation of silver powder (99.9%) using
GLAD.10,11,3336 Before the deposition, Si substrates were
ultrasonically cleaned in acetone. Si substrates were mounted
on the sample holder and was inclined in such a way that the
normal of the sample surface made a very high angle
(a 85) with respect to the direction of the incident vapourflux. The substrate temperature was regulated to control the
morphology of the grown Ag nanorods arrays. A customized
substrate holder with a heater and controlled supply of liquid
nitrogen was used to maintain the substrate temperature of
133 K. The temperature was measured with an accuracy of61 K using PT100 temperature sensor placed closed to the
substrate. The chamber pressure during deposition was better
than 2 106 Torr. For reference conventional Ag thin filmswere also grown with the normal incidence (a 0) of vaporflux on Si substrates. The surface morphology of the resulting
nanorods was investigated by scanning electron microscope
(SEM, ZIESS EVO 50).
In order to make the Ag nanorods surface hydrophobic,
the AgNR samples were coated by dipping the AgNR sub-
strates in a solution of 1 mM HDFT prepared in 30 ml etha-
nol for different time varying from 15 min to 60 min. After
a)Author to whom correspondence should be addressed. Electronic mail:
0003-6951/2014/104(2)/023107/4/$30.00 VC 2014 AIP Publishing LLC104, 023107-1
APPLIED PHYSICS LETTERS104, 023107 (2014)
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incubation, the samples were removed from the solution,
gently rinsed with de-ionized (DI) water and dried with a
gentle nitrogen blow. To determine the static contact angle,
water droplets of 5 ll volume were deposited on AgNR sam-
ples. The images of the droplets on samples were captured
using CMOS camera equipped with a magnifying lens. The
contact angle on the Ag nanorods was measured by analyz-
ing the water droplets images with ImageJ software
(National Institute of Health, USA). The contact angle meas-urements were repeated five times at different positions of
each sample. For SEF measurements, 1 mM aqueous solution
of Rhodamine 6G (Rh6G) in DI water was prepared. The
droplet of 5 ll volume of this aqueous dye solution was de-
posited on AgNR samples and was allowed to dry in an am-
bient temperature. The fluorescence measurement was done
using ISS PC1 spectrofluorometer equipped with a 300 W
Xe arc lamp at room temperature (RT) using 511 nm excita-
tion wavelength.
GLAD is a physical vapour deposition technique where
the deposition flux is incident on a substrate with a large
vapour angle (>75) with respect to the surface normal.37
Due to the shadowing effect during growth GLAD produces
AgNR arrays inclined in the direction of vapour flux. The
SEM micrographs of AgNR samples grown at temperature at
313 K and 133 K are shown in Fig.1. It can be observed from
the SEM images that there is a drastic contrast in the surface
morphology of AgNR grown at 133 K and 313 K. The sub-
strate temperatureTssignificantly affects the morphology and
in particularly the size and lateral distribution of Ag nano-
rods. The variation in the size and distribution of AgNR were
calculated in terms of nanorod diameter and nanorod density
(nanorods/cm2). It was found that there was not much varia-
tion in nanorod density (1.3 108 nanorods/cm2 at 313 K to
1.8 108
nanorods/cm
2
at 133 K) but the nanorod diameterdecreases for the low temperature Ts 133K depositedAgNR from 172 nm to 63 nm. Another important difference
is the presence of porous nanostructures in the low tempera-
ture (LT) deposited Ag film, whereas the RT, Ts 313K, de-posited AgNR arrays appear to be solid and more rod like.
The measured contact angle h, on bare AgNR substrates was
found to be 107.16 3 and 134.862.5 for the RT and LT
AgNR substrates, respectively. The superhydrophobic metal-
lic surfaces can be obtained by coating a monolayer of low
surface energy materials like fluorinated compounds. The
AgNR samples were coated with HDFT for different time
varying from 15 min to 60 min. The water contact angle val-
ues were found to increase with the increase in the coatingtime of the HDFT molecules deposited on AgNR substrates
until a critical time was reached after which the water contact
angleh values remained almost unchanged. For example, for
the deposition time of 15 min,hreaches a value of 134.862
and 162.06 2 for RT and LT grown AgNR samples, respec-
tively. However, when the coating time was increased to
30 min, h reaches to a maximum contact angle (hmax) value
attainable on LT AgNR sample of 164.162 and that for the
RT grown AgNR sample hmax was 142.262. Further
increase in the coating time has no effect onh and it remains
almost constant as shown in Fig.2. This is the optimum coat-
ing time for AgNR with HDFT after which no significant
change in the contact angle was observed. The HDFT coating
made the Ag nanorods surface hydrophobic but change in
their surface morphology was not observed after the HDFTcoating (see supplementary material42).
Self assembled monolayers, such as HDFT, are ordered
assemblies ofmolecules that form spontaneously on surface
via adsorption.38 The HDFT surface is nonpolar and the sul-
phur head-group attached to the substrate via covalent bond-
ing promotes close-packing leading to a monolayer covering
the substrate, the tail group serves for the functionalization
purposes to control interfacial properties of the monolayer.
Dipping AgNR substrates in a solution of HDFT supplies a
monolayer of highly fluorinated hydrophobic molecules low-
ering the surface energy and apparently increasing the con-
tact angle.
According to Cassie and Baxter model, the creation ofair gaps because of the roughness can keep the droplet float-
ing thereby increasing its contact angle. The increase in con-
tact angle is given by the relationship39
cos h0 fcos h1 1; (1)
whereh0 is the observed contact angle, h is Youngs contact
angle, and f is the solid fraction on which the droplet sits.
Hence, we can see that the smaller the solid fraction larger
the apparent contact angle.
The decrease in the average nanorod diameter and pres-
ence of porosity decreases the solid fraction due to the
increase in volume of the air entrapped in between the gapsFIG. 1. SEM image of silver nanorods grown on Si substrate at (a) 313 K
and (b) 133 K.
FIG. 2. Variation of water contact angle (h)with HDFT coating time for Ag
nanorods grown at room temperature (313K) and low temperature (133 K).
023107-2 Kumaret al. Appl. Phys. Lett.104, 023107 (2014)
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of the rough structures of LT deposited AgNR substrates.
The presence of air in place of a solid surface simply reduces
the effective surface energies responsible for spreading of
water on the surface and hence improving the hydrophobic-
ity of the considered surface. This composite structure of air
and solid combination along with the presence of low surface
energy components on the roughened surface reduces the af-
finity of water to the surface and thus increases the contact
angle. Therefore, increase in water contact angle value maybe attributed to the rough nanoscale morphological pattern
obtained on these surfaces as well as the presence of low sur-
face energy fluorinated species present on these surfaces.
The superhydrophobic (having hmax value) AgNR sam-
ples grown at 133 K were employed for further SEF studies.
Fig. 3 shows the variation in the peak intensity of fluores-
cence of Rh6G molecule deposited on HDFT coated LT
grown AgNR samples as a function of coating time. The in-
tensity of the fluorescence signal was initially amplified with
an increase in the coating time and then it decreases with the
coating time. As we have discussed that the contact angle
was also found to increase with HDFT coating time, the
increase in the peak intensity may be attributed to the
increase in the contact angle from 134 to 164. For the
enhancement factor (EF) measurements the fluorescence
spectra of Rh6G molecules on both AgNR and reference
substrates were collected. The conventional Ag thin film
grown at RT was considered as the reference substrate for
SEF measurements. The fluorescence intensity was found to
be increased on the AgNR samples. However, it can be
noticed that the fluorescence intensity was observed to be
much higher on the HDFT coated superhydrophobic AgNR
sample compared to the bare AgNR sample. The SEF
response of AgNR samples canbe understood quantitatively
by measuring the EF as follows:
40
EF IsubstrateIbackgroundIreference Ibackground
; (2)
where Isubstrate is the fluorescence intensity on AgNR sub-
strate, Ireference is the fluorescence intensity on reference
(conventional Ag thin film) substrate, and Ibackground is the
background intensity of the spectra. The calculated SEF
enhancement factors of HDFT coated superhydrophobic
AgNR and bare AgNR samples are shown in Fig. 4.
Interestingly, it can be noticed that the HDFT coated AgNR
samples offer almost 3 times greater SEF enhancement fac-
tor compared to bare AgNR samples. This observed rise inEF clearly suggests that the superhydrophobic HDFT coated
AgNR arrays makes a better and highly sensitive SEF active
substrates. This significant amplification in the SEF intensity
of Rh6G can be explained on the basis of superhydrophobic
condensation effect.31,32 When a droplet of a diluted solution
is put on a substrate which is not superhydrophobic then the
droplet will wet the surface and in turn spread out the dis-
solved fluorescent molecules over a larger area. In case of
the superhydrophobic substrate, the contact area between the
droplet and the underlying surface is highly reduced and
when the droplet is allowed to evaporate it progressively
reduces its volume and contact area during evaporation with-
out changing its quasi-spherical shape. Accordingly, the dis-
solved molecule or compound in the droplet that was
initially diluted becomes more and more concentrated and
localized after the evaporation.30,41 At the end of evapora-
tion, when the droplet reaches a condition of instability it
collapsed and the solute get deposited in a confined region
which results in the amplification of the fluorescence signal.
Hence, by using superhydrophobic surfaces the molecules
can get concentrated over a small area to carry out molecular
detection using plasmonic surface enhancement of electro-
magnetic field in the vicinity of metallic nanostructures.
In summary, we have fabricated HDFT coated superhy-
drophobic AgNR substrates for SEF application with contactangle 16462. For AgNR deposited at correspondingly
lower substrate temperature of 133 K, the nanorods were
observed to have smaller diameter of 63 nm compared to
172 nm for the RT (313 K) grown Ag nanorods. The high
contact angle of the LT deposited AgNR is a manifestation
of increase in the porosity and hence increase in the area of
FIG. 3. Variation in peak intensity with HDFT coating time. The normalized
SEF intensities of the strongest peak with different coating time of
Rhodamine 6G. The t 0 corresponds to an uncoated Ag nanorodssubstrate.
FIG. 4. EF measured on bare and HDFT coated Ag nanorod samples with
respect to a conventional Ag thin film. Both the samples were deposited at
133 K substrate temperature.
023107-3 Kumaret al. Appl. Phys. Lett.104, 023107 (2014)
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air entrapped in between the gaps of the nanorods because of
thinner Ag nanorods. The HDFT coated superhydrophobic
AgNR arrays exhibited 3-fold fluorescence signal enhance-
ment than the bare AgNR sample and the signal was found
to increase with increase in the contact angle. These highly
sensitive superhydrophobic SEF active AgNR arrays sub-
strates may offer a potential application such as trace analy-
sis and biosensing.
The author (S.K.) is thankful to IIT Delhi for providing
research fellowship. This research was funded by DST, India
Grant Nos. SR/S2/CMP-13/2010 and RP02395 Nanoscale
Research Facility, IIT Delhi.
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See supplementary material at http://dx.doi.org/10.1063/1.4861836 for
SEM images of bare and HDFT coated Ag nanorods.
023107-4 Kumaret al. Appl. Phys. Lett.104, 023107 (2014)
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