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Sensors andActuatorsB 225 (2016) 498503
Contents lists available at ScienceDirect
Sensors and Actuators B: Chemical
journa l homepage: www.elsevier .com/ locate /snb
Low temperature and large-scale growth ofZnO nanoneedle
arrays with enhanced optical and surface-enhanced
Raman scattering properties
Yu-Cheng Chang
Department of Materials Science and Engineering, FengChiaUniversity, Taichung, 40724, Taiwan
a r t i c l e i n f o
Article history:
Received 11 August 2015
Received in revised form
10 November 2015
Accepted 12 November 2015
Available online 24 November 2015
Keywords:
Nanoneedle
Aqueous chemical growth
Antireflection
Photocatalytic performance
Surface-enhanced Raman scattering
a b s t r a c t
Large-scale ZnO nanoneedlearrayshave been grown on four-inch silicon wafers with ZnO seed film by an
aqueous chemical growth method at a low growth temperature and short reaction time. The volumes of
1,3 diaminopropaneplay an important role in controlling the dimension and optical emission properties
ofZnO nanoneedle arrays, which exhibit a very prominent green emission and weak UV emission from
defect and band gaps in the cathodoluminescence spectrum, respectively. The ZnO nanoneedle arrays
with large alignment variations display broadband and omnidirectional antireflection properties from
the gradual index profile, and can provide a higher surface-to-volume ratio and stronger defect emission,
which results in a peak photocatalytic performance at a light irradiation of10W UV. The appropriate Ag
sputtering durations on the ZnO nanoneedle arrays have been optimized to yield the greatest surface-
enhanced Raman scattering effect in the rhodamine 6G molecule. The ZnO/Ag composite arrays provide
a facile, high enhancement, low detection limit and low cost fabrication, which shall be of significant
value for practical applications ofother SERS sensing systems.
2015 Elsevier B.V. All rights reserved.
1. Introduction
Zinc Oxide (ZnO) is one of most promising oxide materials,
which has attracted considerable interest due to its unique phys-
ical properties, such as its direct and wide band gap (3.37eV),
n-type semiconductor, largeexciton binding energy (60meV),high
electron mobility (100cm2 V1 s1), and piezoelectricity [13].
It is an important functional oxide, exhibiting high photore-
activity, near-UV emission, visible light transparency, biosafety,
and biocompatibility [4,5]. ZnO nanostructures have great poten-
tial for application in ultraviolet (UV) lasers [6,7], light-emitting
diodes [810], thin-film transistors [11,12], field emission (FE)
devices [13,14], solar cells [15], photocatalysis [4,16], and piezo-
nanogenerators [17,18].
ZnO nanostructures have be synthesized by various methods,
such as metal organic chemical vapor deposition [19], molecu-
lar beam epitaxy (MBE) [20], physical vapor deposition (PVD)
[21,22], pulsed laser deposition [23], and thermal evaporation
[24,25]. However, these methods generally require high temper-
ature, involve complicated equipment, and have a low yield [5].
Tel.: +886 424517250x5345; fax: +886 424510014.
E-mail address: [email protected]
The aqueous chemical growth (ACG) method is more attractive
attributed to its low cost, low temperature and feasibility for
industrial-scale fabrication [4,16,26]. Previous works on ACG pro-
cesses have been controlled to grow different morphologies by
adjusting reaction conditions, including pH [27,28], precursor con-
centrations [29], temperature [30], and surfactants [3133], etc.
Recently,ACGmethods have been developedfor fabricationof ZnO
nanostructures in various geometrical morphologies, including
nanowires [34,35], nanorods [29,36], nanotubes [37], nanopagodas
[4,26], nanoneedles [30], nanoplates [4,38], nanoparticles [39], and
nanoflowers [27], etc. Among them, ZnO nanoneedles can provide
for sharp curvatures of tips, which are expected to be of partic-
ular importance in field emissions [40], photocatalysis [41], and
optical properties [30,42]. However, there are fewer reports about
lowtemperature and large-scale growthof ZnOnanoneedle arrays
with high performance antireflective, photocatalytic, and surface-
enhanced Raman scattering properties.
The present work has synthesized well-aligned ZnO nanonee-
dlearraysby theACGmethodon four-inchsilicon waferswith ZnO
seed film. The appropriate volumes of 1,3-diaminopropane (DAP)
can be used to grow the highest aspect ratio of ZnO nanonee-
dle arrays at a relatively low growth temperature of 80 C for
1.5h. Hexamethylenetetramine plays an important role in inhibi-
ting theinfluenceofhigh pHvalueswith largedimensions. TheZnO
http://dx.doi.org/10.1016/j.snb.2015.11.053
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nanoneedle arraysexhibita very weak UVemissionandverystrong
green emission from a defect in the cathodoluminescence spec-
trum. The ZnO nanoneedle arrays have good geometric structures
forantireflectioncoatings,whichdisplaybroadbandreflectionsup-
pression from 4001950nm. ZnOnanoneedle arrays can provide a
higher surface-to-volume ratio and better stability against aggre-
gation, resulting in greater photocatalytic activity. In addition, ZnO
nanoneedle arrays have good geometric structures for deposition
three-dimensional Ag nanoparticles, which lead to high perfor-
mance surface-enhanced Raman scattering (SERS) detection. The
present work can provide insight into further structural design for
nanostructured optical and SERS applications.
2. Experimental
2.1. Synthesis
A Si (001) wafer was cleaned ultrasonically for 10min in
ethanol.A thin filmof zinc acetate wasthencoatedon thesubstrate
byspinninga layer of solutionof 5mM zincacetate dihydrate (98%
Aldrich) in ethanol and repeating for ten times. 510nm thick ZnO
seed film was produced after annealing at 300 C in air for 20min
[4,43]. The ZnO nanoneedle arrays were grown by an ACG methodin 100mLof aqueous solution containing 10mM equimolar zinc
nitrate hexahydrate (98% Aldrich) and hexamethylenetetramine
(99% Aldrich) (HMTA), with the addition of different volumes of
1,3-diaminopropane (98%, Alfa Aesar) (DAP). The substrate with
ZnO seed film was pasted at the side of a sealed bottle containing
the above solution and heated to about T= 80 C for1.5h.
2.2. Characterization
The morphology of nanostructures was examined with a field
emission scanning electron microscope (FESEM) using a JEOL
JSM-6500F SEM operating at 10kV accelerating voltage. A JEOL-
2010 transmission electron microscope (TEM) operating at 200 kV
was used to examine the microstructures. The crystalline phaseof the ZnO nanostructures was determined using the X-ray
powder diffraction method (Shimadzu XRD-6000, CuK1 radia-
tion (= 0.1505nm)). The cathodoluminescence (CL) spectra were
acquired with an electron probe microanalyzer (Shimadzu EPMA-
1500) attached to a SEM. CL spectra were accumulated in a single
shotmodewithinanexposurerateof 1nm/s.All theCL spectrawere
taken at room temperature. The reflection spectra were obtained
with a Hitachi Model U-4100spectrophotometer. The degradation
of methyleneblue solution wasused to evaluate thephotocatalytic
activity of ZnO nanoneedle arrays. The methylene blue solutions
were exposed to a 10W UV lamp. For the photocatalytic activity
evaluation, the concentration of photodegraded methylene blue
was recorded by a Hitachi U-2900 UVvis spectroscopy. Ion sput-
tering (EMITECH KSC7620) was used to deposit Ag nanoparticles
on the surface of ZnO nanoneedle arrays. The Raman spectra were
performed by Confocal Raman Microscope (HORIBA, LabRAM HR)
at room temperature in thebackscattering configuration. The light
source was a He-Ne laser emitting a wavelength of 632.8nm.
3. Results and discussion
3.1. Evaluation of ZnO nanoneedle arrays
Fig. 1ad show the cross-sectional SEM images depicting the
vertical ZnO nanoneedle arrays grown from equimolar (10mM)
zinc nitrate and HMTA, and the different volumes of DAP solu-
tion by an ACG method at the growth temperature of 80 C
for 1.5h. The volumes of DAP were 0.25, 0.5, 0.75, and 1mL,
Fig.1. Thecross-sectionalSEM images of theZnO nanoneedlearraysweregrownon
the silicon substrates with ZnOseed filmat differentvolumes of DAP. The volumes
ofDAPare(a) 0.25,(b) 0.5, (c)0.75,and(d) 1mL,respectively.(e) Theaveragelength
ofZnOnanoneedle arrays as a function of thevolumes of DAP.
respectively. The lengths of ZnO nanoneedles gradually increased
with an increase in DAP volumes, as shown in Fig. 1e. The aver-
age lengths of ZnOnanoneedles were 0.36, 1.29, 1.99, and5.07m,
respectively. Andthemediumdiameters of ZnOnanoneedles were
82.39.4,55.510.4, 53.916.7,and66.514.1nm, respectively.
In addition, the aspect ratios (length /diameter) of ZnO nanonee-
dleswere4.4,23.2,36.9,and76.2, respectively.TheZnOnanoneedle
arrayshad thelongest lengthand highestaspect ratiosat a DAPvol-ume of 1mL. In general, the solubility of ZnO in an alkali solution
was found to increase with an increase in the alkali concentration
and temperature [44]. The pH value turned from 6.94 to 11.45 by
the addition of DAP (1mL) in the growth solution. If the volumes
of DAP are higher than 1mL, the solution becomes too alkaline
to restrain the growth of ZnO nanoneedle arrays. The excessive
amount of DAP not only influenced the growth of ZnO nanonee-
dle arrays, but also etched the ZnO seed film. On the other hand,
appropriate volumes of DAP lead to the growth of ZnO nanoneedle
arrays with long length and high aspect ratio.
The seed film has been found to be beneficial for fabricating
ZnO nanowire or nanorod arrays with a wafer-scale production
by the ACG method with a neutral pH value [45]. And in order to
ensure that the alkaline condition would not influence the growththeuniformityof ZnOnanoneedlearraysfora four-inchwaferscale,
highconcentrations(20mM)ofzinc acetatedihydrate were used to
prepare a thicker ZnO seed film for the growth of ZnO nanoneedle
arrays. Inaddition,a bigger reactionchamberanda copiousreaction
solution were neededto grow aligned andregular ZnOnanoneedle
arrays over a large area. Fig. 2a shows that ZnO nanoneedle arrays
successfully covered a four-inch Si wafer. SEM images taken from
several four-inch samples revealed that entirewafer canbe grown
with highly uniform andaligned ZnOnanoneedle arrays, as shown
in Figs. 2b and c. The medium diameters and average lengths of
ZnO nanoneedles were 71.216.8nm and 4.76m, respectively.
In addition, the average density of ZnO nanoneedle arrays was
4.3109 cm2. AndthedimensionsofZnOnanoneedlearrayswere
notchangedby anincrease insizeofthe reactionchamberor adding
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Fig. 2. (a) A photography and (b-c) SEM images of ZnO nanoneedle arrays were
grown on a four-inch silicon wafer at different locations, magnifications, and tile
angles(0 or20).(d) Theplan-viewSEMimageof ZnOnanoneedle arrayswasgrown
from 10mM zinc nitrate and 1 mLDAPon the silicon substrate with ZnOseed film.
Fig. 3. (a)TEM image of a ZnO nanoneedle arraysin Fig. 1(d). (b)HRTEMimageand
corresponding SAED pattern confirming the single crystallinity of a ZnO nanonee-
dle in (a). (c) XRD spectrum of ZnO nanoneedle arrays was grown on the silicon
substrates with ZnOseed film.
to theamountofreactionsolution.Fig.2d showsthat theplan-view
SEMimage depicting theZnOnanoneedle arrayswere grown from
10mM zinc nitrate and 1mLDAP on the silicon substrate withZnO
seed film. The medium diameters and density of ZnO nanoneedles
were 329.8130.4nm and 3.7108 cm2, respectively. When the
reaction solution wasonly zinc nitrate andDAP, thedimensions of
ZnOnanoneedle arrays appeared non-uniform and aggregate. This
phenomenon is attributed to HMTA acting as both a long chain
polymer and a nonpolar chelating agent at low reaction temper-
atures. HMTA is preferentially attached to the nonpolar facets ofthe ZnO crystal, in turn restraining the access of Zn2+ ions to them
and leaving only the polar [00 1] face for epitaxial growth [46,47].
Therefore, HMTA acts a shape-inducing polymer surfactant to con-
trol the dimension of ZnO nanoneedle arrays.
Fig. 3a shows a TEM image of a ZnO nanoneedle (in Fig. 1d)
with a length of 1136nm and tip diameter of about 8nm. The
high-resolution TEM image taken from part of an individual ZnO
nanoneedle and the corresponding SAED pattern is shown Fig. 3b
andthe inset,respectively, whichalso shows thesame [01 0] zone-
axis SAED pattern. Both the HRTEM image and diffraction pattern
indicate that the ZnO nanoneedle is single-crystalline and grown
in the [00 1] direction. The crystal perfection of the ZnO nanonee-
dle arrays was also investigated by X-ray powder diffraction. The
XRD pattern of nanoneedles grown on the ZnO seed film is shown
Fig. 4. Cathodoluminescencespectra of ZnO nanoneedle arrays weregrown on the
silicon substrates with ZnOseed filmat thedifferent volumes of DAP. The volumes
ofDAP were0.25, 0.5, 0.75,and 1mL, respectively.
in Fig. 3c. A strong and sharp diffraction peak corresponding to
the (00 2) crystal plane of ZnO indicates that the preferred growth
direction of the ZnO nanoneedles is in the [00 1].
3.2. Optical properties of ZnO nanoneedle arrays
To investigate the optical properties of ZnO nanoneedle arrays,
cathodoluminescence (CL) spectroscopy was employed. All the CL
spectra were takenat room temperature.Fig. 4 shows that CL spec-
tra of ZnO nanoneedle arrays were grown in different volumes of
DAP. The volumes of DAP were 0.25, 0.5, 0.75, and 1mL, respec-
tively. From 0.25 to 0.75mL, the intensityof theband gapemission
did not change with an increase in the volume of DAP. However,
the intensity of green emission had a tendency to increase with an
increase in thevolume ofDAP. Themaximumgreenemissionpeaks
were 556, 560, 565, and 573 nm, respectively. This result is accor-
dant with the currently accepted model that the green emission
arises from the recombination between holes trapped at the sur-
face defect andelectrons trapped at theoxygenvacancy [30]. With
an increase in the volumes of DAP, the maximum peaks of greenemission evinced a red shift. The red shift shall be attributed to
thereverse quantum confinement effectarising from theincreased
lengths of nanoneedles. In some previousworks,the energyshift of
nanostructures with dimensions far beyond thequantum confine-
ment regime is ascribed to the surface effect due to the increased
surface-to-volume ratio [4,16,36,48]. The ZnO nanoneedle arrays
exhibit the strongest UV and defect emission at DAP volumes of
1 mL. The surface oxygendeficiencies are electron capture centers,
which can be used to enhance the photocatalytic activity of ZnO
nanostructuresbyreducingtherecombinationrateof electronsand
holes [16,49]. The significant defect emission property and high
surface-to-volume ratio of ZnO nanoneedles shall be beneficial to
photocatalytic applications.
ZnO nanostructures have been very suitable for using efficientantireflection coating layers, which are attributed to their high
transparency, appropriative refractive index, and feasible fabrica-
tionprocess [42,50]. Herein, thespecular reflectancewas measured
todeterminethe antireflectiveproperties ofZnOnanoneedlearrays
for wavelength of 3501900nm, as shown in Fig. 5. The incident
angle was fixed at 5 relative to normal samples in the measure-
ment. When compared the ZnO seed film and ZnO nanoneedle
arrays at different volumes of DAP revealed the importance of
morphology on antireflection coating layer performance. The ZnO
nanoneedle arrays (1mLDAP) displayed the lowest reflectance in
the broad range of wavelength. The morphology of ZnO nanonee-
dle arrays exhibited sharp tips and long lengths, which denotes
a gradual decrease in the refractive index from the surface of Si
substrate to the ambient air, resulting in the best antireflection
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Fig. 5. The reflection spectra of the different ZnO nanostructures were grown on
the silicon substrates.
properties. Broadband antireflection characteristics are generally
correlated with a graded refractive index profile [51]. In addition,
the small bumps at 890nm on the curve come from the detector
change during the data collection of the equipment. These find-
ings show that ZnO nanoneedle arrays with the broadband and
omnidirectional antireflectioncoatings can greatly benefittheper-
formance of optical and electric devices, such as light-emitting
diodes and photovoltaic cells.
3.3. Photocatalytic properties of ZnO nanoneedle arrays
Methylene blue (MB) is selected as a representative organic
pollutant to evaluate the photocatalytic performance of the ZnO
nanoneedle arrays under 10W UV light irradiation. The ZnO
nanoneedle arrays were grown on a 1cm2cm silicon substrate
as a photocatalytic sample. The photocatalytic degradation of MB
solution under UV light irradiation was conducted to evaluate the
photocatalytic activity for ZnO nanoneedle arrays grown by the
different volumes of DAP, as shown in Fig. 6a. The decrease in
absorbance at a wavelength of 664nm was observed with the
increase of irradiation time andDAPvolumes. TheZnOnanoneedlearrays (at 1mLDAP) exhibited the highest photocatalytic activ-
ity in the decomposition of MB. This phenomenon coincides with
the highest aspect ratio and strongest defect emission of ZnO
nanoneedle arrays (at 1 mLDAP), and provides direct evidence in
demonstrating that a strongdefect emission anda high surface-to-
volume ratio are beneficial to enhance the photocatalytic activity.
Fig. 6b shows the photocatalytic efficiency of the different ZnO
nanoneedle arrays, whichwere grownin thereactionsolutionwith
(Fig. 1d) or without HMTA (Fig. 2d) by an ACG method. The ZnO
nanoneedle arrays (with HMTA) exhibit a high surface-to-volume
ratio (smalldimension andhigh density), resulting ina higherpho-
tocatalytic efficiency.
In order to confirm the stability and reusability of ZnO
nanoneedle arrays, cyclic experiments were used to evaluate thephotodegradation efficiency of MB. The MB solution with the ZnO
nanoneedle arrays (1mL) on a silicon substrate was illumined
under UV light for 3h and rinsed with de-ionized water to remove
the residual MB, and dried under an N2 purge. This substrate was
then immersed into a fresh MB solution with the same concentra-
tionfor anothercycleof photodecomposition.Over tencycles, these
experiments show that the degradation rate was almost constant,
confirmingthat ZnOnanoneedlearraysareinherentlystableduring
prolonged photocatalytic reactions, as shown in Fig. 6c. After ten
cycles, theZnOnanoneedle arraysmaintained a high reusability of
95.6%. SEM examination of this substrate after ten cycles suggests
that the nanoneedles appearance and density will not undergo
any change. Therefore, ZnO nanoneedle arrays are expected to
have a long service life as photocatalysts with high efficiency and
Fig. 6. The MB normalization concentrations (from the optical absorbance mea-
surements at 664nm) in the solution with ZnOnanoneedle arrays substrates were
grown by (a) the different volumes of DAP and (b) with or without HMTA versus
the irradiationtime of UV light, respectively. (c)Themaximumabsorptionintensity
at 664nm as function of photodecompositioncycles forthe ZnOnanoneedle arrays
(1mLDAP) under UV light irradiation for 3h at room temperature.
durability. Furthermore, ZnO nanoneedle arrays that are grown
on a silicon substrate simplify the recycling process, making ZnO
nanoneedle arrays steady and economical photocatalysts.
3.4. Surface-enhanced Raman scattering properties of ZnO
nanoneedle arrays
Recently, ZnO has received special attention due to its
excellent performance for supporting chemical enhancement of
surface-enhancedRaman scattering (SERS) substrates [52,53]. ZnO
nanoneedle arrays exhibit good geometric structures for deposit-
ing Ag nanoparticles, with better stability against aggregation for
the applications of SERS substrates. Rhodamine 6G (R6G) was
chosen as the probe molecule owing to its well-established vibra-
tional features. [54,55]. Figs. 7 a-e show the SERS spectra of R6G
solution (1106 M) dispersed on the ZnO nanoneedle arrays
with different Ag-sputtering durations. The Ag-sputtering dura-
tions were 30, 60, 90, 120, and 150s, respectively. The strong and
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Fig. 7. SERS spectra of R6G (1106 M) absorbed on the ZnO nanoneedle arrays
withdifferent Ag-sputteringdurations. TheAg-sputteringdurations were(a) 30, (b)
60, (c) 90, (d) 120, and (e) 150 s, respectively.
Fig. 8. (a) The SERS signals at 1657cm1 versus the Si or ZnO nanoneedle arrays
were depositedwith differentAg-sputteringdurations. (b) TheSERS signals of ZnO
nanoneedle arrays with an Ag-sputtering duration of 60 s at 1657 cm1 versus the
differentconcentrations of R6G.
medium-strong Raman bands at 1365, 1514, 1578, and 1657 cm1
arise from the totally symmetric modes of in-plane C C stretching
vibrations [55]. An obvious trend shows that the intensity of the
Raman signal at 1657cm1 decreased strongly with an increase in
theAg-sputteringdurationsfrom60150s. ZnOnanoneedlearrays
with Ag-sputtering duration of 60s exhibited the maximum SERS
signals. The change of SERS intensity is attributed to the differ-
ent coverage and sizes of Ag nanoparticles on the ZnO nanoneedle
arrays obtained from different Ag-sputtering durations. When the
Ag-sputtering durations were longer than 60 s, the Ag nanoparti-
clesappearedtheaggregationandreductionthe SERSsignals.These
results confirm that theAg-sputtering durations play a crucial role
in determining the coverage and sizes of Ag nanoparticles on the
ZnO nanoneedle arrayswith highest SERS enhancement.
Fig. 8a shows the Raman intensity at 1657cm1 obtained from
the different Ag-sputtering durations on the Si or ZnO nanonee-
dle arrays, respectively. It is clearly observed that the signals of
ZnO nanoneedle arrays with different Ag-sputtering durations are
much higher than Si with different Ag-sputtering durations. The
Ramanintensityof Si isdecreasedwithan increase inAg-sputtering
durations. This phenomenon is attributed to the occurrence of
aggregation with an Ag-sputtering duration longer than 30s. In
addition, the SERS enhancement factor (EF) of the ZnO nanonee-
dle arrays with Ag-sputtering durations of 30s and 60s is about
14.6 and 67.2 times greater than Si with an Ag-sputtering dura-
tion of 30s. The different Ag-sputtering durations on the Si and
ZnOnanoneedle arraysfor thedetection of R6G(1657 cm1)canbe
statistically evaluated in Table 1. The SERS activity of the ZnO/Ag
composite arrays is higher than only Ag nanoparticles, which can
be explained by the electromagnetic enhancement mechanism as
a result of surface plasmon resonance excitation of Ag nanopar-
ticles, and chemical enhancement effects of ZnO [52]. To further
reveal the good SERS enhancement effects of the ZnO nanoneedle
arrayswithAg sputtering for60 s,theRamanintensityat1657cm1
is obtained from the different concentration of R6G, as shown in
Fig. 8b. The SERS signals at1657cm1 are indeed found to increase
with an increase in the concentration of R6G. The peak remains
clearly observable in the R6G solution with concentrations as low
as109 M. This indicates that theZnO/Agcompositearraysas SERS
substrates provide strong Raman signals of R6G. The fabrication of
ZnO/Ag composite arrays is facile, low cost, highly enhanced, and
with a low detection limit (109 M), which shall be advantageous
in applications for other SERS sensing systems.
4. Conclusions
VerticallyalignedZnO nanoneedlearrayshavebeen synthesized
on a Si wafer with ZnO seed film using a facile ACG method with
a low reaction temperature and a short reaction time. The dimen-
sions andoptical emissionproperties of ZnOnanoneedle arraysare
effectively controlled by the volumes of DAP. The ZnO nanonee-
dle arrays exhibit very strong and broad green emission from
defectin thecathodoluminescence spectrum.The sharp tips of ZnO
nanoneedlearraysprovideexcellent impedancematchingbetween
Si and air through a gradual reduction of the effective refractive
index away from the surface, resulting in superior antireflection
property over a greater range of wavelength. ZnO nanoneedlearrays have shown a structure-induced enhancement of photo-
catalytic performance by higher surface-to-volume ratio, which
exhibits a muchbetter photocatalyticproperty for thephotodegra-
dation of MB in 10W UV light irradiation. The ZnO nanoneedle
arrays withappropriate Ag-sputtering durationhaveexhibited the
highest SERS activity for R6G detection, suggesting their great
potentialas a convenientSERSsubstrateforbiosensorapplications.
Table 1
The SERS singles ofR6G (1657cm1) obtained on theSi andZnOnanoneedle arrays with thedifferent Ag-sputtering durations.
Ag-sputtering durations 30 s 60 s 90 s 120s 150s
SERS enhancement (Si) 50378
SERS enhancement (ZnO nanoneedle arrays) 7320846 338203814 301505138 178803526 4950975
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