Sensors & Actuators: A.

Physical 347 (2022) 113932

Contents lists available at ScienceDirect

Sensors and Actuators: A. Physical

journal homepage: www.journals.elsevier.com/sensors-and-actuators-a-physical

Gold nanoparticles are capped under the IRMOF-3 platform for in-situ
surface-enhanced Raman scattering technique and optic fiber sensor
Nguyen La Ngoc Tran a, b, 1, Bach Thang Phan b, c, 2, Hanh Kieu Thi Ta a, b, 1, Tran Thi Kim Chi d, 3,
Bui Thi Thu Hien d, 3, Nguyen Tran Truc Phuong a, b, 1, Chi Cuong Nguyen b, c, 2,
Tan Le Hoang Doan b, c, *, 2, 4, Nhu Hoa Thi Tran a, b, **, 1, 5
a
Faculty of Materials Science and Technology, University of Science, Ho Chi Minh City, Viet Nam
b
Vietnam National University, Ho Chi Minh City, Viet Nam
c
Center for Innovative Materials and Architectures (INOMAR), HoChiMinh City, Viet Nam
d
Institute of Materials Science, Vietnam Academy of Science and Technology, Hanoi, Viet Nam

A R T I C L E I N F O A B S T R A C T

Keywords: Integrating noble-metal and organic-inorganic hybrid crystalline porous materials for Raman signal augmenta­
Surface-enhanced Raman scattering tion is crucial for surface-enhance Raman spectroscopy. This study effectively generated gold nanoparticles /
Nanostructures metal-organic frameworks (Au NPs/IRMOF-3) hybrids. The activity of Au NPs/IRMOF-3 double component
Biochemical sensor
substrate was significantly enhanced under localized surface plasmon resonance (LSPR) because the hot electrons
Optical fiber sensor
Rhodamine B
produced on Au NPs surface were incorporated with IRMOF-3 and utilized the porous structure to capture the
analyte. Development much hot spots of great significance for surface-enhanced Raman scattering (SERS)
technique, herein, we developed an Au NPs/IRMOF-3-based nanosensor for rhodamine B (RhB) sensing by using
in-situ SERS technique. X-ray diffraction (XRD) spectrometry, surface morphology analysis, optical properties,
and energy-dispersive X-ray (EDX) spectroscopy were used to examine the layer-by-layer deposited substrate.
The Au NPs/IRMOF-3 multilayers generated chemical and electromagnetic amplification of Raman signals of
Rhodamine B at a low concentration and high enhancement factor. In the presence of dopamine molecules, due
to the strong specific affinity between the modified surface out-layer of fiber sensor and the target molecules,
resulting in the obvious change of the optical power transmission signals, which can be used for dopamine
sensing with high sensitivity and stability (limit of detection is 1.42 × 10-18 M with a wide linear range from 10-
17
to 6 × 10-8 M of dopamine). The Au NPs/IRMOF-3 nanosensor can be used as an ideal platform for real
applications, especially for some gases or low-weight molecules in the future.

1. Introduction nondestructive, less sample consumption, and noninvasive analysis, and

specificity) while addressing the inherent shortcoming of weak Raman
Surface-enhanced Raman spectroscopy (SERS) is an ultrasensitive scattering caused by small cross-sections [1–3]. SERS is growing in
vibrational spectroscopic analytical technique that inherits the advan­ popularity due to its numerous applications in materials characteriza­
tages over conventional Raman spectroscopy (quick reaction, tion [4], and biomedicine [5], amongst many others. Finding and

* Corresponding author at: Center for Innovative Materials and Architectures (INOMAR), HoChiMinh City, Viet Nam.
** Corresponding author at: Faculty of Materials Science and Technology, University of Science, Ho Chi Minh City, Viet Nam.
E-mail addresses: latran429@gmail.com (N. La Ngoc Tran), pbthang@inomar.edu.vn (B.T. Phan), ttkhanh@hcmus.edu.vn (H.K.T. Ta), chittk@ims.vast.ac.vn
(T.T.K. Chi), hienbtt@ims.vast.ac.vn (B.T.T. Hien), nguyentrantrucphuong9568@gmail.com (N.T.T. Phuong), nccuong@inomar.edu.vn (C.C. Nguyen), dlhtan@
inomar.edu.vn (T.L.H. Doan), ttnhoa@hcmus.edu.vn (N.H.T. Tran).
1
Faculty of Materials Science and Technology, University of Science, Vietnam National University, Ho Chi Minh City, Vietnam.
2
Center for Innovative Materials and Architectures (INOMAR), Vietnam National University, Ho Chi Minh City, Vietnam.
3
Institute of Materials Science, Vietnam Academy of Science and Technology, Hanoi, Vietnam.
4
https://orcid.org/ 0000–0001-6312–9571
5
https://orcid.org/ 0000–0002-1530–2402

https://doi.org/10.1016/j.sna.2022.113932
Received 7 August 2022; Received in revised form 24 September 2022; Accepted 2 October 2022
Available online 4 October 2022
0924-4247/© 2022 Elsevier B.V. All rights reserved.
N. La Ngoc Tran et al.
establishing great SERS substrates is essential for practical application
because method properties are heavily reliant on active substrates,
which primarily include (i) plasmonic materials (Au, Ag, Cu) substrates
based on electromagnetic enhancement (EM) [6] and (ii) other materials
substrates based on chemical enhancement (CM) [6]. Investigating
novel materials and employing them to logically manufacture
high-performance substrates are thus necessary to advance its devel­
opment and application. SERS substrates have evolved dramatically
over the last few decades, from a few single-component plasmonic ma­
terials [7,8] to diverse multi-component composites [9–11]. Combining
new materials (such as solid-phase microextraction materials, multi­
functional materials [12], chemical enhancement materials [13], and
plasmonic nanoparticles into high-performance SERS substrates has
been shown to improve SERS performance in practical applications.
Metal-organic frameworks (MOFs), which have large surface areas,
rapid absorption, and enrichment abilities, and a chemical enhancement
effect, provide a great opportunity to absorb target molecules onto or
near the surface of plasmonic nanoparticles to achieve highly effective
enhancement and improve detection. MOFs are crystalline materials
that self-assemble from the coordination of polydentate ligands to metal
clusters [14–16]. MOF structures and properties can be uniquely
adjusted by customizing the metal clusters and ligands, in addition to
being simple to synthesize. MOFs have extraordinary properties [17–19]
due to their unique structure, which includes (i) permanent nanoscale
porosity with large internal surface areas and ultralow densities, (ii)
uniform structured cavities that provide a molecular sieve effect, (iii)
exposed active sites of metal ions or ligand groups with specificity, and
so on. Due to their distinct framework architectures and exceptional
characteristics, MOFs offer significant potential for SERS research. Much
further, different MOF-based substrates have been used for SERS ap­
plications, including single-component substrates [20,21],
double-component plasmonic nanoparticles-MOF substrates [22–24],
and multi-component substrates [25,26].
We fabricated a double component on a glass substrate by layer-layer
deposition of self-assembled gold nanoparticles monolayers and the
outermost IRMOF-3 layer, dubbed the Au NPs/IRMOF-3 multilayer. In
this work, 2-aminoterephthalic acid units are linked through octahedral
[Zn4O]6+ clusters to generate IRMOF-3. IRMOF-3 has a single amino
group on each of its carboxylate linkers, and these linear and octahedral
building blocks combine to form primitive-cubic lattices. IRMOF-3
possesses great properties of MOFs, such as large high surface areas
for rapid molecular enrichment, uniform framework pore for size-
selectivity, and exposed active sites for sensitive detection. While Au
NPs can produce EM enhancement by creating more “hot spots” on the
local surface to amplify SERS signals of target molecules, then IRMOF-3
monolayer outside deposited to contribute rapid electron transport and
enhanced chemical attraction to the target molecule through the inter­
action of π − π stacking at the ligands of IRMOF-3, resulting additional
SERS signals enhancement. Besides, the rational designation and con­
struction of Au NPs/IRMOF-3 substrate can greatly meet the demand for
SERS detection. MOFs hybrids with plasmonic nanoparticles can be
made via non-covalent interactions, such as encapsulation [27,28],
layer-by-layer deposition [29], and in situ growth [30]. These ap­
proaches make use of noncovalent interactions between MOFs and the
hybridizing species by trapping the species within the pores, stacking
them on top of the parent materials, or growing crystals in situ with the
species. Therefore, the non-covalent modification enables the distinct
properties of the IRMOF-3 and hybridizing materials (Au NPs/IRMOF-3
multilayers) to work synergistically in the resulting hybrids while
requiring less synthetic effort than covalent modification.
Herein, we demonstrate Au NPs/IRMOF-3 multilayer substrate ap­
plications for high SERS-active detecting of low concentrations of
rhodamine B (RhB) and ultra-sensitive with dopamine through an op­
tical fiber sensor. In the LSPR-based optical biosensor fabrication, Au
NPs were produced through the seed-mediated growth approach. The
limit of detection (LOD) of sensor structure is lower and simpler than
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Sensors and Actuators: A. Physical 347 (2022) 113932
reported before. For example, our study gives SERS performance about
10 times higher than the SERS substrate Ag/rGO/Au for detecting RhB
(LOD = 10 nM), which was investigated by Aiping Liu et al. [31].
Furthermore, our Au NPs/IRMOF-3 based SERS substrates for RhB
detection outperformed 100 times the W18O49 nanowire film reported
by Wang et al. [32] that the W18O49 nanowire film assembled using a
three-phase interface method and the SERS detection limit of RhB can
reach 10-7 M. Moreover, different dopamine concentrations cause the
refractive index to change near the interface of the active fiber sensing
area. LSPR is sensitive to the effective refractive index change and leads
to the optic power transmission shift. LSPR occurs when the frequencies
of incident photons match the collective oscillation of electrons at the
surface of metallic nanoparticles [33]. Thus, a low-cost and easily
fabricated fiber-optic probe is proposed to monitor the change in
transmitted light power in an output signal detector. The Au nano­
particles and IRMOF-3 layer were loaded on the fiber core as an LSPR
sensing region. The results show that this fiber-optic LSPR sensor can
provide online monitoring of the signal of optic transmission in situ and
is ultra-sensitive when there is a change in the effective refractive index.
The intensity shift in the LSPR sensor has a good linear relationship with
the dopamine concentration and the output light signal recorded. In
addition, our optical fiber sensor gives a fast response, is real-time,
label-free, and occurs at room temperature, presenting great potential
in practical applications. Using a plasmonic fiber-optic sensor with Au
NPs/IRMOF-3 platforms in our study to detection of dopamine also
achieved a LOD approximately 105 times higher than the limit detected
through the graphene functionalized layer, reported by Wanjun Hu et al.
[34]. The performance of our fiber sensor system is 1011 times greater
than the maximum detection limit of the fiber optic dopamine sensor
employing green synthesized silver nanoparticles, as reported by
Rithesh Raj et al. [35]. In addition, the LSPR sensing area based Au
NPs/IRMOF-3 on fiber interface gave a super-sensitivity to dopamine
109 times higher than the deposition method to obtain a three-layer
composite of gold nanoparticles, choline, and graphene quantum dots
on a carbon fiber microelectrode, reported by Lili Yang et al. with an
estimated limit of detection of 1.616 nM [36]. Therefore, the structure
of Au NPs/IRMOF-3 multiplayer opens horizons for application to LSPR
functions in biosensors via dopamine sensor research using optic fiber
sensors.
2. Experimental
2.1. Material and reagent
Gold (III) chloride trihydrate (HAuCl40.3 H2O, 99%, Sigma-Aldrich,
USA), sodium citrate tribasic dihydrate (Na3Ctr, 99% Sigma-Aldrich,
USA), sodium hydroxide (NaOH, Guangdong Guanghua Sci-Tech,
China). Zinc acetate dihydrate (Zn(OAc)20.2 H2O, 98%, Sigma-
Aldrich, USA), 2-aminoterephthalic acid (H2BDC-NH2, 99%, Acros,
USA), Hexadecyltrimethylammonium bromide (CTAB, 99%, Acros,
USA), polyvinylpyrrolidone (PVP, average mol wt. 40000, Sigma-
Aldrich, USA), (3-Aminopropyl) triethoxysilane (APTES, 99%, Sigma-
Aldrich, USA), and succinic acid (SA, 99%, Sigma-Aldrich, USA),
ethanol (EtOH, 99.5%), methanol (MeOH, 99.5%), and N,N-
dimethylformamide (DMF, 99.8%) were provided from Fisher, USA.
Polydimethylsiloxane (PDMS) and Sylgard 184 were from Dow Corning
Co., USA. The sensor is linked together via aligning a multimode optical
fiber with a core diameter of 200 µm (numerical aperture of 0.37,
JFTLH-Polymicro Technologies). De-ionized (DI) water (Thermo Scien­
tific Easypure II, Göteborg, Sweden) produced in the Center for Inno­
vative Materials and Architectures (INOMAR), Vietnam National
University, Ho Chi Minh City (VNU-HCM) was used for all preparations.
ISOLAB Laborgeräte GmbH. Eschau (in Germany) provided the micro­
scope glass slides (soda-lime glass, chemical composition: SiO2, Na2O,
CaO + MgO as 75 ± 5; 15 ± 2; 10 ± 2 wt%, respectively.
N. La Ngoc Tran et al. Sensors and Actuators: A. Physical 347 (2022) 113932

2.2. Synthesis of metal-organic framework-3 (IRMOF-3) 3. Results and discussion

IRMOF-3 was prepared by magnetic stirring at room temperature for
30 min with solutions of 10.5 mg 2-aminoterephthalic acid, 10 mg
cetyltrimethylammonium bromide (CTAB), 7.5 mg poly­
vinylpyrrolidone (PVP), and 35 mg zinc nitrate hexahydrate in dime­
thylformamide (DMF). These compounds were conducted to solvent
exchange with DMF and methanol successively to remove excess metal
salts and linkers from their pores, and the residual methanol was
removed from the materials in a vacuum. Before proceeding with further
investigations, we checked the crystallinity of their materials by
measuring their powder X-Ray diffraction patterns after completing the
production and solvent exchange of IRMOF-3.
2.3. Fabrication of sensor substrates
In Scheme 1, after generating hydroxyl groups (-OH) on the clean-
glass surface for 2 min with an oxygen plasma machine (CUTE-1MPR,
Femto Science Inc., Korea), it was silanized with 3% APTES. The study
[37] referred to the synthesis of Au NPs. Following that, a strong elec­
trostatic force was used to immobilize Au NPs on the amine-modified
sample for 16 h. The Au NPs modified glass was then
carboxyl-functionalized for 1 h at 80 ℃ in a 0.4 M SA acid solution.
Finally, the substrate surface was immersed in IRMOF-3 solution for the
duration of the experiment (2, 3, and 6 days).
3.1. Characterization of Au NPs/IRMOF-3 multilayers
The substrate’s SERS characteristic is closely related to its synthesis
conditions. Thus, ultraviolet-visible (UV–vis) absorption spectroscopy is
used to undertake a qualitative evaluation of solution synthesis optical
absorption characteristics, and the findings are shown in Fig. 1. The
IRMOF-3 material has the absorption peak of H2BDC-NH2 at 335 nm
[38], which is related to ligand-to-metal charge transfer and, thus,
unique optical absorption endowing IRMOF-3 with the opportunity to
efficiently apply for SERS sensor via variable coordination chemistry. In
this approach, gold nanoparticles produced by reducing gold (III)
chloride trihydrate are critical for improving the Raman signal benefits
from their distinctive localized surface plasmon resonance. The nano­
particles development method allows for more precise control of Au NPs
features such as absorbance size and wavelength, as well as the synthesis
of single. Anisotropic noble metal nanocrystalline structures often
exhibit one or more plasmon resonance bands, indicating that the
spectra of Au seed and Au NPs peak at around 523 nm and 524 nm,
respectively. (Fig. 1) [39,40]. The band found at around 524 nm in Au
NPs is connected to surface plasmon resonance [39]. Nonetheless, the
absorption band in these Au seeds and Au NPs broadened with a tiny red

2.4. Characterization

The materials were characterized by utilizing UV–visible spectros­

copy (V-730 visible/ NIR, JASCO, Tokyo, Japan), powder X-ray
diffraction (PXRD, Bruker D8 Advance diffractometer, λ = 1.54178 Å),
and field emission scanning electron microscope (FESEM, Hitachi
S4800, USA). The presence of the surface functional groups such as
hydroxyl, carboxyl, and amino was investigated by water contact angles
(WCAs, Phoenix 300, Surface Electro-Optics). The Raman spectra of the
analyte were recorded by using micro-Raman spectroscopy (Horiba
Xplora One, Horiba scientific, Horiba Ltd.) with excitation by a green
laser (532 nm wavelength, 25 mW power source, 10X objective micro­
scope, 10 s accumulation time). The instrument was calibrated by a
silicon wafer with a Raman band at 520 cm-1.

Fig. 1. UV–vis absorption spectra corresponding to Au seed, Au NPs, and

IRMOF-3 solutions.

Scheme 1. Illustrates the functionalization on silica surface to immobilization of IRMOF-3 and Au NPs/IRMOF-3.

3
N. La Ngoc Tran et al.
change in the LSPR, possibly due to the material size effect [41]. We can
conclude from UV–vis absorption data that Au NPs and IRMOF-3 solu­
tions were well regulated and simple to make, and that they can be used
in a variety of applications such as SERS and optic fiber sensor activity
testing.
WCA measurements were taken after each step of functionalization
to explore the bare glass surface change, as shown in Fig. 2a. Due to the
formation of functional -OH groups on glass by the oxygen plasma
machine, the water contact angle was immediately decreased from 43.6◦
to 11.5◦ . The wetting angle increased to 72.4◦ after APTES functional­
ization, indicating the presence of a hydrophobic layer on the surface.
Then, with an angle of 76.8◦ , it was established that the Au NPs layer
coated glass was more hydrophobic than the amine-modified surface.
The extremely low contact angle of 20.3◦ demonstrated that the hy­
drophobic coating of the Au NPs substrate became hydrophilic after 1 h
of succinic acid treatment etching, owing to the surface remaining with
COOH-terminals on the Au NPs substrate. We observed an increase in
contact angle to 68.1◦ after immersing the glass in IRMOF-3 solution.
These results are explained by forming the IRMOF-3 s layer via the as­
sociation of the -COOH group of modified glass and the -NH2 group of
H2BDC-NH2 ligands. Attributed to the prevalence of hydrophobic Au
NPs, the contact angle of Au NPs/IRMOF-3 multilayer substrate is
greater than that of IRMOF-3 monolayer on glass (as 25.2◦ ). The change
in surface wetness in WCAs suggested that -OH, -NH2, and -COOH
groups were successfully produced on the wafer surface, as shown by
XRD in Fig. 2b-d [42–44].
To verify the crystallinity of materials, XRD patterns measuring be­
Fig. 2. (a) WCA of substrates. XRD patterns of (b) the IRMOF-3 films with various immersion times, (c) Au NPs monolayer, and (d) Au NPs/IRMOF-3 multilayer.
4
Sensors and Actuators: A. Physical 347 (2022) 113932
tween 2θ of 5◦ and 80◦ were used. The XRD patterns formed with an
ascending sequence of immersion times ranging from 2 to 6 days, which
has exhibited the (200), (220), and (400) lattice surfaces correspond to
the typical diffraction peaks at 6.8◦ , 9.7◦ , and 13.6◦ , respectively, and
are indexed for the IRMOF-3 by the stated values (Fig. 2a) [45,46].
Furthermore, it is said that the crystalline structure of IRMOF-3 is
reserved based on functionalization with other groups [47]. The
strength of this peak, however, increases with an increasing immersion
time of the substrate in IRMOF-3 solutions. This indicates that the film
crystallinity increases with denaturation time, showing that the mono­
layer has been stabilized by a stable chemical link at the substrate sur­
face between the -NH2 group of ligands and the modified-glass -COOH
group. The next studies used a three-day immersion time to improve
stability and reduce sensor assembly time. The XRD pattern clearly
shows the presence of Au in the monolayer of Au NPs on glass and
identified at 2θ as 38.1◦ , 44.3◦ , 64.5◦ , and 77.6◦ , which are attributed to
Bragg’s reflection of face-centered cubic (fcc) Au (Fig. 2c) [48]. For Au
NPs/IRMOF-3 multilayer substrates, the diffraction peaks of Au NPs
observed at 2 θ = 38.1◦ and 44.2◦ are related to the crystal planes of Au
(111) and Au (200), respectively; additionally, the presence of IRMOF-3
peaks was preserved, as shown in Fig. 2d.
Fig. 3a-c depicts a FESEM micrograph of as-prepared Au NPs and
IRMOF-3, with an enlarged image and scale bars of 200 nm and 500 nm.
We examined the effects of size, shape, and population of Au NPs in the
Au capping process on the surface of a sensor substrate using FESEM
images taken after a 16-hour immersion duration. The Au NPs after the
Au capping technique is monodispersity spherical in shape with a
N. La Ngoc Tran et al.
Fig. 3. FESEM images of (a) Au NPs, (b) IRMOF-3, and (c) Au NPs/ IRMOF-3 multilayer with scale bar 500 nm and inset scale bar 200 nm. (d) EDX spectra for Au
NPs/IRMOF-3 platforms on the glass substrate and the corresponding elemental composition.
diameter of around 28 nm and are equally positioned with no heavy
clustering of nanoparticles (Fig. 3a). For double component substrates
constructed using the layer-layer structure, the uniform distribution is
repeated. The -NH2 group of IRMOF-3 forms a connection with the
-COOH group of the modified substrate to immobilize the Au NPs layer
in preparation for the second capping procedure. According to Fig. 3b,
IRMOF-3 particles were hexahedrons (cube and cuboid), had a some­
what uniform structure, and were concentrated within a 50 nm range
[45,49]. The FESEM picture and EDX spectrum of the Au NPs/IRMOF-3
multilayer are given in Fig. 3c,d. The EDX analysis indicates the exis­
tence of all constituent elements in the nanostructure in Fig. 3d. It is
clear that the Au NPs/IRMOF-3 nanostructure is composed of 0.83 wt%
of zinc and 10.46 wt% of gold. Besides, both 0.23 and 0.95 at% of zinc
and Au were found in the final multilayer platforms due to the experi­
mental conditions, which include all elements other than IRMOF-3
crystal structures such as carbon (32.56 wt% and 48.58 at%) and oxy­
gen (29.24 wt% and 32.75 at%). Furthermore, double component ma­
terials were evenly and steadily dispersed across the substrate surface. In
general, the nucleation–growth pathway and a magnetic stirrer
approach for Au NPs and IRMOF-3 were successful in the production of
multilayer sensor substrates.
3.2. SERS activities of Au NPs/IRMOF-3 substrates
The molecule RhB was chosen as a guest analyte for this food dye has
the potential to seriously harm human health. The structure of RhB in­
cludes delocalized large π bonds, so the π-π interaction mechanism be­
tween RhB and the bridging molecules of the IRMOF-3 with a benzene
ring could be thoroughly and conveniently evaluated. LSPR of gold
nanoparticles effect increases electric field density creating a strong
electric field region; moreover, RhB is trapped close to Au NPs surface
through the nanopores of the IRMOF-3, which enhances dispersion
Raman radiation of RhB emitted. Because Au NPs are frequently applied
as SERS substrates and can amplify signals using an electromagnetic
field, they are a great candidate for RhB detection [50]. The porous
structure of IRMOF-3 electromagnetic has the benefit of aiding the
confinement of the molecule to reside near the sturdy surface of Au NPs
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Sensors and Actuators: A. Physical 347 (2022) 113932
under LSPR excitation. Therefore, a charge-transfer mechanism like
hydrogen bonds or aromatic ring contacts in connection to stacking
interaction may also be used by the IRMOF-3 to offer the chemical
augmentation of the Raman signal [51,52]. In order to detect RhB by
SERS, Au NPs/IRMOF-3 platforms were used (Fig. 4a).
An impressive SERS amplification may be seen when the laser’s
excitation wavelength is close to the LSPR band of Au nanostructures
[53]. By using a 532 nm laser, the SERS characteristics of RhB on Au
NPs/IRMOF-3 substrates were examined. Rhodamine B has character­
istic Raman peaks at 622 cm-1 (xanthene ring puckering mode),
1075 cm-1 (C-H out-plane bending), 1197 cm-1 (C–C bridge band
stretching and aromatic), 1273 cm-1 (H–C–H wagging vibration),
1357 cm-1 (Aromatic C–C bending), 1433 cm-1 (C–C, C = C–C stretching
and bending vibration), 1505 and 1561 cm-1 (Aromatic C–H bending),
1647 cm-1 (Aromatic C–C bending and C– – C stretching), and 1594 cm-1
(C = N in-plane symmetric stretching vibration) [54–56]. The
enhancement factor of a substrate was then calculated by the following
equation:
ISERS CRaman
EF = ×
IRaman CSERS
where ISERS and IRaman are the Raman intensities of the RhB molecules at
1647 cm-1 on the SERS Au NPs/IRMOF-3 substrate and normal Raman
signals, respectively, to quantify SERS performance CSERS and CRaman
refer to the concentration of RhB molecules within the laser spot excited
by Au NPs/IRMOF-3 substrate and normal Raman spectroscopy,
respectively [57,58]. By using the formula, the enhancement factor was
determined to be 6.54 × 109 with a 10-9 M low concentration detected.
To test the suggested SERS substrate’s sensitivity, RhB concentrations
ranging from 10-9 M to 10-3 M were used. The peak intensity of RhB at
1647 cm-1 changes linearly with the different RhB concentrations.
The key issues that must be addressed for practical implementation
are the high uniformity and reproducibility of SERS substrates. The SERS
substrate’s dependable performance is ultimately determined by the
homogenous distribution of nanostructured materials on multilayer
platforms. In Fig. 5, the SERS spectra were measured at six randomly
selected points on the Au NPs/IRMOF-3 substrates to test the uniformity,
N. La Ngoc Tran et al.
Fig. 4. SERS spectra (a) and calibration curve (b) for RhB at different concentrations.
Fig. 5. SERS spectra of rhodamine B molecules at 10-6 M from six random site
on the Au NPs/IRMOF-3 platforms.
and the relative standard deviation values were calculated. At the
Raman peaks 1647, 1357, 1273, and 622 cm-1, the relative standard
deviation (RSD) values for 10-6 M RhB are 3.12%, 6.34%, 11.13%, and
14.69%, respectively. (Fig. 6) The minimal RSD values for RhB detection
show that the Au NPs/IRMOF-3-based SERS substrate has good spot-to-
spot uniformity. The small RSD values in the uniformity and reproduc­
ibility tests can be attributed to the uniform distribution of Au NPs and
IRMOF-3, which is given a good experimental operation. To further
Fig. 6. The average data of SERS intensity were collected at six different po­
sitions on the Au NPs/IRMOF-3 substrates at specialty Raman shift of RhB and
RSD values at 622, 1273, 1357, and 1647 cm-1 respectively (inserted Figure).
6
Sensors and Actuators: A. Physical 347 (2022) 113932
evaluate the stability of the Au NPs/IRMOF-3 hybrid structure, the
Raman spectra of RhB molecules on the same "hotspot" of the SERS-
active substrate were recorded following the storage time of 30, 60,
and 90 days after fabrication. The results showed that after prolonged
storage, the random sites on the SERS platforms still maintained the
characteristic peaks of the RhB molecule with intensity at 1647 cm-1
obtained 65.3% compared to signal Raman intensity of the substrate
right after fabrication. (Fig. 7) The foregoing results show that the Au
NPs/IRMOF-3 substrate has achieved the required homogeneity,
reproducibility, and stability as a SERS substrate for practical
application.
3.3. Operating efficiently of optical fiber sensors
Our previous report [59,60] designed and implemented real-time
optical fiber biosensor measurement. Fig. 8 demonstrates optical
power transmission as a function of dopamine concentration. To test the
effectiveness of the optical fiber optic sensing system, dopamine solution
was created at concentrations ranging from 10− 17 to 6 × 10− 8 M. We
successively injected a variety of concentrations of dopamine solution
within each concentration range, with each injection being preceded by
a de-ionized water rinse of the surface. The optical power transmission
quickly increases until the concentration as 4 × 10− 8 M [59,61].
Accordingly, a transmission change may be caused by a rise in liquid
concentration [59]. As it becomes more concentrated, the liquid clad­
ding’s effective index rises, increasing the amount of optical power that
can be transmitted through the interface between two fiber outputs.
Because this sensor’s working concept is based on the medium’s
changing refractive index, it can detect various proteins with various
refractive indices and produce various signals. The -COOH groups on the
Au NPs/IRMOF-3 coated sensing surface made it simple to immobilize
dopamine molecules. The signal increase happened over a time of about
1 min, although it seemed to increase rapidly. This showed that the
dopamine molecules initially fixed on the surface via amino-carboxyl
coupling and then colonized the space immediately above it. It was
possible to deduce that the sensor’s index sensitivity was higher in an
area nearer to the surface. At lower dopamine concentrations, we saw
the signal saturation that followed an increase, but the signal increases
more slowly at higher dopamine concentrations. This may have
occurred because a higher dopamine concentration increased the in­
tensity of the dopamine-dopamine coupling and decreased the
amino-carboxylic coupling, which reduced the number of dopamine
molecules immobilized on the surface. At least three times, a 1 min
recording of the average signal intensity with the error bar was made for
each concentration. The coefficient of variation was then calculated to
be less than 1%, demonstrating a good level of reproducibility. Due to
N. La Ngoc Tran et al. Sensors and Actuators: A. Physical 347 (2022) 113932

Fig. 7. (a) SERS spectra for rhodamine B molecules at 10-6 M detected by Au NPs/IRMOF-3 substrates following storage time and (b) relationship between Raman
intensity and storage time after 30, 60, and 90 days.

Fig. 8. (a) The optical fiber biosensor system image with PSMS microfluidic device, (b) the fiber sensor responds to the change in dopamine concentration from 0 to
6 × 10-8 M and (c) enlarged scale from 10-17 to 10-14 M.

7
N. La Ngoc Tran et al. Sensors and Actuators: A. Physical 347 (2022) 113932

Table 1 Data availability

Comparison of performance for the dopamine biosensors.
Substrates LOD (M) Linear range (M) Reference The data that has been used is confidential.
Other methods
Acknowledgments
Fluorescence 1.18 × 10− 7
1.3×10− 7 − [62]
3.9×10− 7
Enzyme-based biosensor 6×10− 7
1.5×10− 5 − [63] This study is supported by Vietnam National University Ho Chi Minh
86.5×10− 5 City to Center for Innovative Materials and Architectures (Laboratory for
Catalytic 2.3 × 10− 9
10− 8 − 7×10− 7 [64] Optics and Sensing) under grant NCM2019-50-01
chemiluminescence
Visible photoelectric 6.7 × 10− 9
2 × 10− 8
− 10− 4 [65]
chemistry
Optical fiber sensor
Notes
Silver nanoparticles 2 × 10− 7 2 × 10− 7 [35]
Graphene 1.66 × 10− 13 10− 13 − 10− 8 [34] The authors declare no competing financial interest.
Au NPs/IRMOF-3 1.42 × 10− 18 10− 17 − 6 × 10− 8 Our work

the signal’s ability to vary considerably and instantly as analyte con­
centration changes, this sensor was given a high sensitivity rating. The
fiber optical LSPR biosensor has a calculated limit of the detection value
of 1.42 × 10− 18 M, which is higher than that of other sensors, as shown in
Table 1 demonstrates its outstanding efficiency. Therefore, given this
performance, our sensor can be acknowledged as a workable tool for
biosensing.
4. Conclusion
In summary, we have produced the high-performance SERS substrate
based on the IRMOF-3 layer adorned on Au NPs platforms. The practi­
cality of the suggested SERS substrates for the sensitive detection of RhB
was examined after using a quick and simple procedure. UV–vis, XRD,
FESEM, and EDX studies were used to determine the structural and
surface characteristics of the suggested SERS substrate. Self-assembled
Au NPs monolayers are provided a large number of active hotspots on
the surface sensor. Besides, IRMOF-3 platforms have supported electron
transport quickly and created molecular trapping sites by unique porous
architecture, resulting in enhanced chemical and electromagnetic to
increase the Raman signal of target molecules. Then, we studied the
various concentration of the sample, and the SERS sensitivity and uni­
formity of the substrate have been confirmed by using RhB as a mo­
lecular probe to explore. The research shown above shows that the
synthesized SERS substrate offers a broad linear range for detecting RhB
with an analytical enhancement factor of approximately 6.54 × 109.
Eventually, a variety of dopamine concentrations are adopted to test the
efficiency of an optic fiber sensor, resulting in markedly sensitive to the
transmitted optical power signal at extremely small changes in the
concentration of the dopamine. The Au NPs/IRMOF-3-based LSPR
sensor is opened the future way for biosensors.
CRediT authorship contribution statement
N.L.N.T.: Conceptualization, Methodology, Writing – original draft
preparation, Data curation, Formal analysis; B.T.P; T.T.K.H; N.T.T.P;
C.C.N.: Data curation, Formal analysis; T.T.K.C., B.T.T.H., T.L.H.D.:
Data curation, Methodology, N.H.T.T.: Supervision, Funding acquisi­
tion; Investigation; Methodology, Writing – reviewing and editing,
Funding acquisition.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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Ms. Nguyen La Ngoc Tran is an M.Sc student in materials
sciences and received a B.Sc degree (2021) in thin film and
nanomaterials sciences, faculty of Materials Science from the
University of Science, Vietnam National University Ho Chi
Minh City. She is studying the Master’s course in the faculty
of Materials Science and Technology from the University of
Science, Vietnam National University Ho Chi Minh City with
a major in Materials Science. She is working in Optics and
Sensing group at the faculty of Materials Science and Tech­
nology, University of Science, Vietnam National University
Ho Chi Minh City. Her main research interests are in Surface-
enhanced Raman spectroscopy, optical biosensors, and their
applications in biomedical optical fiber sensors.
Prof. Bach Thang Phan received a BSc degree from the
University of Science, Hochiminh city, Vietnam with a major
in Applied Physics. He received a Ph.D. degree in 2009 at the
School of Advanced Materials Science and Engineering,
Sungkyunkwan University, Korea. He is now a director in the
Center for Innovative Materials and Architectures, Vietnam
National University, Hochiminh city. His research interests
are thermoelectric thin film materials, thin film process, and
properties of nanolaminate oxide electronics, memristive
biosensors, and magnetic materials.
MSc. Hanh Kieu Thi Ta received a BSc degree (2004) and M.
Sc degree (2010) in physics from the University of Science,
Ho Chi Minh City, Vietnam with a major in Applied Physics
and Optics. She is studying Doctor degree in Materials Sci­
ence from the VNUHCM-University of Science. Now, She is
working at the faculty of Materials Science and Technology,
University of Science, Vietnam National University Ho Chi
Minh City. Her main research interests are in thermoelectric
thin film materials, thin film processes, optical biosensors,
bionano-photonics, memristive biosensors, and magnetic
materials.
Dr. Tran Thi Kim Chi received B.Sc degree (2000) in Phys­
ics, Faculty of Physics from University of Science, Vietnam
National University Hanoi and M.Sc degree (2002) in Mate­
rials Science from International Training Institute for Mate­
rials Science (ITIMS), Hanoi University of Science and
Technology. She completed her D.Phil from the Institute of
Materials Science (IMS), Vietnam Academy of Science and
Technology (VAST) in 2011. Now, she is working at the
Laboratory of Electron Microscopy, Institute of Materials
Science (IMS), Vietnam Academy of Science and Technology
(VAST). Her main research interests are in studying the
properties of micro and nano materials; synthesis, and opti­
mization of synthesis parameters for quantum dots and
nanomaterials which emit visible luminescence oriented for optical biolabeling.
enhanced fluorescence for PCR, optical biosensors, bionano-photonics, and their appli­
cations in biomedical optical fiber sensors.
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Sensors and Actuators: A. Physical 347 (2022) 113932
M.Sc. Bui Thi Thu Hien received B.Sc degree (2016) in
materials sciences, faculty of Physics from University of Sci­
ence, Vietnam National University, Hanoi, and M.Sc degree
(2020) in Solid State Physics from Graduate University of
Science and Technology, Vietnam Academy of Science and
Technology. Now, She is working at the Institute of Materials
Science, Vietnam Academy of Science and Technology. Her
main research interests are in Electron Microscopy Sciences,
optical materials, photocatalytic materials, and their
applications.
Ms. Nguyen Tran Truc Phuong received B.Sc degree (2021)
in thin film and nanomaterials sciences, faculty of Materials
Science and Technology from University of Science, Vietnam
National University Ho Chi Minh City. She is studying the
Master’s course in the faculty of Materials Science and
Technology from the University of Science, Vietnam National
University Ho Chi Minh City with a major in Materials Sci­
ence. Now, She is working at the NTT Hi-Tech Institute,
Nguyen Tat Thanh University, Ho Chi Minh City, Vietnam.
Her main research interests are in surface plasmons reso­
nance (SPR)-enhanced, Surface-enhanced Raman scattering
(SERS), and optical fiber sensors.
Mr. Chi Cuong Nguyen received B.Sc degree (2021) in
biomaterial sciences, faculty of Materials Science and Tech­
nology from University of Science, Vietnam National Uni­
versity Ho Chi Minh City. Now, he is working at the Center
for Innovative Materials and Architectures (INOMAR), Viet­
nam National University Ho Chi Minh City. His main research
interests are in thermoelectric materials.
Dr. Tan Le Hoang Doan received his B.S. degree in honor
program from the University of Science, Viet Nam National
University – Ho Chi Minh City in 2009 and a Ph.D. degree in
Molecular and Nano architecture program from Viet Nam
National University – Ho Chi Minh City in 2017. He was a
postdoctoral researcher at Kyoto University, Japan in 2018.
He is currently working as a senior researcher at the Center
for Innovative Materials and Architectures (INOMAR), Viet
Nam National University – Ho Chi Minh City. His research
interests focus on the design, synthesis, and applications of
porous materials.
Dr. Nhu Hoa Thi Tran received B.Sc degree (2011) in thin
film and nanomaterials sciences, faculty of Materials Science
and Technology and M.Sc degree (2014) in physics and en­
gineering physics from University of Science, Vietnam Na­
tional University Ho Chi Minh City. She completed her D.Phil
from the department of Nano Science and Technology, Col­
lege of BioNano Technology, Gachon University, the Re­
public of Korea in 2018 and performed assistant professor at
the department of Nano-Physics, Gachon University, and the
Republic of Korea (2018). Now, She is working at the faculty
of Materials Science and Technology, University of Science,
Vietnam National University Ho Chi Minh City. Her main
research interests are in surface plasmons resonance (SPR)-