Sensors & Actuators: B.

Chemical 369 (2022) 132391

Contents lists available at ScienceDirect

Sensors and Actuators: B. Chemical

journal homepage: www.elsevier.com/locate/snb

Design and fabrication of an ultra-sensitive Ta2C MXene/Au-coated tilted

grating sensor
Wen Yang a, Yangyang Cheng a, Mingshun Jiang a, *, Shouzhen Jiang b, Runcheng Liu b,
Jiajun Lu b, Lutao Du c, Peilong Li c, Chuanxin Wang c
a
School of Control Science and Engineering, Shandong University, Jingshi Road, 250061, Jinan, China
b
Collaborative Innovation Center of Light Manipulations and Applications in Universities of Shandong, School of Physics and Electronics, Shandong Normal University,
Jinan 250014, China
c
The Second Hospital, Cheeloo College of Medicine, Shandong University, No. 247 Beiyuan Street, Jinan 250033, Shandong Province, China

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

Keywords: Accurate evaluation of trace biochemical molecular signals by fiber-optic sensors is highly challenging. Recently,
Tilted fiber Bragg grating MXene, as one of the most promising 2D materials with unique optoelectronic properties and structural ad­
Surface plasmon resonance vantages, has attracted numerous concerns about the sensitization of optical fiber sensors. This paper proposed
Ta2C MXene
an innovative Ta2C MXene (Ta2C-M) sensitized Au-coated tilted fiber Bragg grating (TFBG) SPR sensor. We
achieved the optimal deposition scheme for Ta2C-M by varying the laser induction time. The introduction of
Ta2C-M brought a 23.3% increase in sensitivity and exhibited an excellent figure of merit (FOM=2586.11 RIU-1)
and linearity (R2 =0.99903). Based on COMSOL, a 3D diversity analysis model was proposed, which validated
the polarization response of the TFBG sensor, the electromagnetic gain of the Ta2C-M coating and enabled the
fitting evaluation of the SPR behavior. The sensitization mechanism of the Ta2C-M coating was further analyzed
utilizing energy band theory based on the Vienna ab initio Simulation Package (VASP). The assessment of two
carcinogenic food additives, Saccharin and BHT, demonstrated the extreme SPR signal resolution and accurate
trace detection performance (10-11 M) of the Ta2C-M/Au/TFBG sensor. These findings indicate that the proposed
sensor will hopefully open new biotechnology, medicine, and food safety detection avenues.

1. Introduction former has the characteristics of high integration, good flexibility,

Sensors based on surface plasmon resonance (SPR) have received
increasing attention as one of the most powerful and essential spectral
graphical analysis techniques, allowing slight alterations in the refrac­
tive index (RI) around a medium visualized by changes in the wave­
length and amplitude of the transmission spectrum [1–3]. Accurately
evaluating the faint fluctuation of RI plays a vital role in biochemical
applications such as bioassay [4,5], energy and environmental protec­
tion [6], food safety [7], etc. Therefore, the need for
ultra-high-resolution and sensitive sensors becomes exceptionally ur­
gent. To date, considerable efforts have been conducted to boost the
detection capability of fiber-optic SPR sensors. Various fiber optic
structures aimed at this objective have been proposed and can be
broadly classified into two categories: mechanically etched “leaky mode
evanescent field” fiber-optic sensors [8–10] and “modulated evanescent
field” fiber optic sensors with complete structures [11–13]. Although the
remote detection, and anti-electromagnetic interference compared with
the traditional prism SPR sensor [14]. However, the evanescent field
prepared by mechanical etching inevitably introduces a loss of optical
energy. Excessive broadening of the SPR signal (tens to hundreds of
nanometers) tends to introduce errors in tracking analysis.
Unlike "leak-mode evaporation field" fiber-optic SPR sensors, TFBG
sensors have a denser surface energy density based on a synergistic
coupling reaction between periodic modulation of the inner core
refractive index and excitation surface plasmon waves (SPWs) [15].
Thus, the dense comb spectra of SPR signals exhibit extremely narrow
absorption peak spreads (0.1 nm) and excellent sensitivity, making them
fabulous for assessing micro- SPR behavior in various fields [16]. Runlin
Wang et al. achieved in situ, real-time and accurate measurements of the
dynamic distribution of electrons and ions and their energy storage ki­
netics inside a battery based on an Au/TFBG sensor [17]. Liu Lanhua
et al. performed an estrogen-specific assay based on an Au-coated TFBG

* Corresponding author.
E-mail address: jiangmingshun@sdu.edu.cn (M. Jiang).

https://doi.org/10.1016/j.snb.2022.132391
Received 30 April 2022; Received in revised form 23 June 2022; Accepted 15 July 2022
Available online 16 July 2022
0925-4005/© 2022 Elsevier B.V. All rights reserved.
W. Yang et al.
sensor with a detection limit as low as 1.5 × 10-3 ng/mL [18]. Fang
Wang et al. used 2-aminoethanethiol (AET) and PMBA-modified Au NPS
for highly selective microselection of glucose [19]. The above studies
have demonstrated the superior detection capability and applicability of
SPPs-based TFBG sensors. A few further illustrate the polarization
pattern and electromagnetic distribution of the TFBG end surfaces.
However, it remains a challenge to study the surface proton response
law, polarization mode, polarization state distribution and transport
required for the coupling state of SPW excitation and periodic modu­
lation of the grating. Moreover, accurate fitting studies of the SPR
behavior of TFBG sensors are even scarcer. This point has a guiding
effect on optimizing the cladding structure of the sensor. Furthermore,
the molecular capability, modifiability, and detection performance of
TFBG sensors with a single SPPs structure are limited.
Two-dimensional (2D) atomic layer materials such as graphene,
MoS2, and Mxene are widely used for sensitization and surface modifi­
cation of optical sensors based on their excellent properties. Especially,
MXene has attracted extensive attention as a novel material with a
ternary MAX phase structure [20]. Its unique layered hexagonal struc­
ture shows a large specific surface, making MXene a perfect molecular
concentrator. Compared with graphene, the MXene surface is rich in
hydrophilic functional groups (-OH, =O, and -F), which exhibit good
hydrophilicity and molecular capture in detecting trace biochemical
molecules [21]. Moreover, the unique broad-band optical absorption
effectively avoids the light source selectivity of the optical sensor [22].
The photoelectric characteristics of MXene are adjustable, which is
achieved by changing the number of layers or surface functional groups
to tune the direct bandgap of the material [23]. These features make
MXene the most sought-after candidate in the SPR field. Yuzhi Chen
et al. used the Ti3C2Tx MXene sensitized fiber optic sensor, which
exhibited excellent detection performance and 30% performance
improvement [24]. Shuaiwen Gan et al. utilized Ti2C MXene
nanosheet-coated SPR sensors to detect Pb2+, Cr2+ and Hg2+ heavy
metal ions and described excellent sensitivities of 3.788 nm/µg/L and
5.308 nm/ng/L, and 2.233 nm/µg/L, respectively [25]. Duo Yi et al.
achieved ultra-sensitive detection of salinity environments (salinity
sensitivity: 5.34 nm/‰) using a Ti3CN MXene coated Mach-Zehnder
interferometer sensor [26]. These studies have validated MXene mate­
rials’ feasibility for optical sensor performance sensitization. However,
existing studies have largely failed to produce uniform and continuous
2D MXene coatings, as excessively thick and inhomogeneous structures
introduce optical energy losses and severely limit their applicability.
There is also a lack of research reports on the sensitization mechanisms
of MXene materials in optical sensors, especially optical fiber sensors.
Inspired by the above, the Ta2C-M/Au/TFBG SPR sensor was
developed by combining the merits of novel 2D Ta2C-M and Au-coated
TFBG. Continuous and homogeneous Ta2C MXene coatings were intro­
duced for surface modification and performance sensitization of TFBG
sensors based on the optimization of photo-deposition conditions. We
demonstrated the excellent SPR behavior of the Ta2C-M/Au/TFBG SPR
sensor and analyzed the sensitization mechanism introduced by Ta2C-M
experimentally and theoretically. The introduction of finite elements
systematically analyzes the SPP polarization state, electromagnetic
distribution and transport response present in the TFBG, and achieves a
fitting evaluation that is highly consistent with the experimental SPR
behavior. Qualitative and quantitative analysis of two carcinogenic food
additives, saccharin and BHT, and detection of trace environments were
presented. We believe that this highly efficient and sensitive TFBG SPR
sensor will pave a promising avenue for detecting biochemical
molecules.
2. Experimental and simulation
2.1. Materials
Ta2C-M material (sheet size: 1–5 µm) was obtained from Yoshiura
2
Sensors and Actuators: B. Chemical 369 (2022) 132391
Nano Co. Deionized water was used as a solvent to prepare a 0.2 g/L
Ta2C-M solution with ultrasound for 10 h. Au was purchased from
Fuzhou yingfeixun photoelectric Co., Ltd. Ethanol was purchased from
Sinopharm Chemical Reagent Co., Ltd. and diluted into solutions with a
refractive index of 1.3600–1.3604. Saccharin and 2, 6-di-tert-butyl-4-
methyl phenol antioxidant 264 (BHT), two common food additives
with carcinogenic risks, were obtained from Lanyu Co., Ltd. Saccharin
and BHT solutions were prepared into 10-12-10-3 solutions with deion­
ized water and ethanol, respectively.
2.2. Preparation of the Ta2C-M/Au/TFBG SPR sensor
TFBG was prepared by modulating the refractive index of the ordi­
nary quartz fiber core using the phase mask method. The mask param­
eters used were as follows: center spacing = 1099.05 nm, mask length =
10 mm, mask height = 15 mm, substrate length = 17.17 mm, substrate
height = 25.4 mm. The modulation tilt angle was 12◦ . The preparation
process was consistent with the previous studies of our research group,
as shown in [27]. A 50 nm Au nanolayer was deposited on both sides of
TFBG components by sputtering under the following deposition condi­
tions: atmospheric pressure = 7 × 10-5 Pa, deposition rate= 0.1 Å/s. The
sensor was placed in a 0.2 g/L solution of Ta2C-M for 150 min under the
excitation of a detection light source, involving a photo-deposition
technique [24]. Special attention was paid to the TFBG sensor to be in
suspension to avoid contact agglomeration at the bottom.
2.3. Experimental setup
The structure and optical detection path of the Ta2C-M/Au/TFBG
SPR sensor are shown in Fig. 1. The sensor was fixed on a poly­
dimethylsiloxane (PDMS) microfluidic chip (parameters: width: 2 µm,
height: 2 µm, length: 3.8 cm). The model number of a microfluidic
peristaltic pump was QHZS-001B. The excitation light source was the
combined light source of ASE-CL-30-M and SLD-1470–10-B. A Yoko­
gawa AQ 63700 spectrometer was used for spectral modulation and
analysis. The VZB-400 thermal evaporation plant was used to prepare
Au film. The cladding structure’s surface morphology and dispersed X-
ray spectroscopy (EDS) were observed by Zeiss Gemini ultra-55 scanning
electron microscope (SEM) equipped with energy sensor. The required
solutions’ refractive index was measured by Abbe refractometer (DR-
A1) at 25 ºC. More detailed morphology and composition were charac­
terized by transmission electron microscopy (TEM, Jem-2100f) and
high-resolution transmission electron microscopy (HRTEM) equipped
with selected area electron diffraction (SAED). X-ray photoelectron
spectroscopy (XPS, Thermo Fisher Scientific 250xi) was used to analyze
the composition and valence state of the sensor surface. A Raman
spectrometer (Horiba lab ram HR evolution 800) was used for Surface-
enhanced Raman spectroscopy (SERS).
3. Results and discussion
3.1. Performance testing and polarization analysis of Au/TFBG sensors
The difference between the S and P polarization spectra in the SPR
transmission mode spectral region (marked by the red dashed box) was
obtained with the ethanol solution (RI: 1.3600–1.3604), as shown in
Fig. 2(a). These “polarization-difference spectra” allow visualization of
smaller shifts due to the resonance’s hyperspectral slope. Linearly
polarized light is emitted with a polarization parallel to the inclined
plane of the inner core (P polarization), and the electric field of the
cladding mode achieves a polarization response in the radial direction
(TM polarization concerning the metal coating) [28]. The evidence for
SPR in this polarized spectrum is the disappearance of the cladding
mode resonance near 1553 nm, which is due to the coupling of the
cladding mode energy to the excited state SPW loss at these.
wavelengths. In contrast, the input polarized light is incident in the
W. Yang et al.
Fig. 1. Schematic diagram of the Ta2C-M/Au/TFBG sensor structure and optical detection path.
other direction. The electric field is aligned with the fiber surface in the
TE direction (S-polarized) with no SPR response. Further, Fig. 2(b) de­
tails the signal polarization response of the SPR labeled region in the P-
polarized state. A distinct signal offset (marked with a red asterisk) is
observed based on the evolution of the effective refractive index of the
cladding mode as the dielectric environment RI changes. And the cor­
responding 1–6 coupling peaks (CP1–6) all show similar response states.
The SPR response equation is shown below [29]:
( )
j j
∧ ∂ neff ,core + neff ,clad njeff ,core + njeff ,clad ∂∧
j
Δλclad, RI = ( + )ΔnRI (1)
cosθ ∂nRI cosθ ∂nRI
where Δλclad,RI is the wavelength response, ∧ is the grating period, and θ
j j
is the tilt angle of the grating. neff ,core , neff ,clad , j are the effective indices of
the core and clad modes, respectively. ΔnRI is the RI change. Since the
j appearance of the SPR signal. The uniform distribution of symmetric
effect of RI on neff,core and ∧ is too weak, it can be approximated to zero
and expressed as:
/ Furthermore, we divided the excited states of SPPs into the compo­
∂njeff ,core ∂nRI = 0, ∂ ∧ /∂nRI = 0
Then, Eq. (1) is transformed into the following equation based on the
approximation treatment [30].
j
∧ ∂neff ,clad
Δλjclad, = ΔnRI
RI
cosθ ∂nRI
The resonant wavelength of the TFBG cladding mode will drift with
the RI based on Eq. (3). Therefore, the changes in RI can be sensed by
measuring the shift in the resonance peak wavelength of the cladding
mode in the transmission spectrum [31]. Moreover, the core-mode
coupling peak exhibits high uniformity manifested by the homogenei­
ty of the color gamut, as shown in Fig. 2(c). The self-reverse coupling of
the fiber core mode provides an absolute temperature reference,
avoiding the influence of environmental factors [32]. However, the
excessive broadening of the labeled SPR signal can easily introduce er­
rors in trace detection. Therefore, it is essential to select an appropriate
response signal. The four dimensions of sensitivity, amplitude response,
linearity and quality factor are used to evaluate the sensor performance,
as shown in Fig. 2(d), (e). The CP2 is used for subsequent sensor
Sensors and Actuators: B. Chemical 369 (2022) 132391
performance evaluation due to the optimal detection performance.
The polarization state of Au/TFBG and the polarization response of
the surface plasma were analyzed based on COMSOL software. Multi­
mode coupling at Bragg wavelengths exhibits the most efficient TM11
order mode in TFBG fibers [33]. The electric field energy bound to the
core region is directed to the non-zero evaporation field at the cladding
boundary. And the cladding external resonant system (Au) is excited by
the modulation effect of the polarization response based on the Z-axis of
the grating inclination [34]. Therefore, the SPPs of the TFBG sensors
have a more substantial field localization effect and more considerable
electric field gain, which couples the energy bound initially to the
cladding to the SPPs and propagates it to the interface between the Au
and dielectric layers [35]. The unique coupling polarization leads to a
sharp change in the transmission spectrum of the TFBG at the wave­
length of the appropriate resonance, which is consistent with the
bright stripes in the grating tilt direction and the polarization distribu­
tion of the cores verify this theory, as shown in Fig. 2(f).
(2)
nents Ez, Ex, and the transmission mode Ey of the light incident plane to
further study the multi-coupling modes based on inclined gratings. (see
Fig. 2(g)-(i)) The excited-state energy distribution of the electric field Ez
component exhibits similar to Fig. 2(f). It is essentially a multimode
coupling response of the polarized beam propagating in the fiber core
(3)
under the modulation effect of the tilted grating, which corresponds to
the polarization mechanism of the P-polarized state. Most importantly,
the electric field energy of the Ez component has an absolute advantage
compared to Ex and Ey, which is consistent with the SPR response
pattern of the TFBG sensor. In addition, the fraction of fiber core Ex
exhibits the asymmetric distribution of top and bottom symmetric sector
areas in the xz-plane due to the asymmetric distribution inside the tilted
grating. The polarization response in the cladding mode exhibits a
unique polarization pattern in which the upper and lower parts differ by
half a phase. The dispersed energy states verify the silencing effect in the
S-polarized state of the TFBG. In addition to the self-directed backward
coupling of the fiber core grating, part of the radially polarized electric
field is coupled as a y-axis polarization mode based on the grating tilt
angle, manifested as the Ey component, which also has a phase delay
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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 2. (a) Differential transmission spectra of P-polarization and S-polarization of Au/TFBG sensor with different ethanol solutions (1.3600–1.3604). (b) Amplified
P- polarization transmission spectra of several CPs near the SPR signal. (c) 2D mapping of the core mode changes of the Au/FBG sensor. (d)-(e) Sensitivity, amplitude
variation, linearity and FOM distribution of the six CPs near the SPR signal, respectively. (f) The polarization state of the Au/TFBG sensor with electromagnetic
distribution under plasmon response (The model see Fig. S1). (g)-(i) the electromagnetic polarization responses of Au/TFBG sensor in an axial and radial direction
(along with the light incident direction) and transmission polarization under plasmon response are shown, respectively (multimedia files).

phenomenon. The multimedia files demonstrate the above phenomena
visually.
3.2. Characterization and Analysis of Ta2C-M/Au/FBG Sensor
Ta2C-M was introduced as a sensitive layer to sensitize the Au/TFBG
sensor based on uniform deposition. Ta2C/Au/TFBG sensor structure is
schematically shown in Fig. 3(a), which demonstrates the loading of
Ta2C as a film-like coating on the Au surface. Moreover, in Fig. 3(b), the
cross-section of Au/TFBG is shown and indicates that the thickness of
the plasmonic layer is 50 nm. The SEM images of.
the Ta2C-M/Au/TFBG sensor under different growth conditions
(50–200 min respectively) were characterized as shown in Fig. 3(c)-(f).
This is a gradual growth process, from mottled surfaces to continuous
membrane-like structures. However, an aggregation effect appeared
around 200 min, which may enhance surface adsorption due to the
variation of the energy density by the Ta2C-M film. Furthermore, the
EDS spectrum in Fig. 3(g) demonstrates the distribution and coexistence
of Ta, Au, C, O elements, and the atomic contents are 25.48%, 51.01%,
15.17%, and 8.34%, respectively. In Fig. 3(hI -hⅣ ), The local composition
of the sample is also measured with EDS elemental mappings, which
reveals the uniform distribution of Ta (blue), C (purple), Au (orange),
and O (light blue) in the coating structure. Moreover, the real-time offset
of the CP2 during the Ta2C-M growth process was counted as Fig. 3(i).
And it exhibits a good long-band shift and amplitude growth before
150 min. The critical wavelength shift is a negligible 0.13 nanometers,
which combines the “positive effect” caused by the Ta2C loading and the
“negative effect” caused by the precipitation of the medium. Subse­
quently, the spectrum appears only as a change in amplitude, which is
the interference brought by the thick coating load. All these features
powerfully demonstrate the composition of the excellent heterostructure
of Ta2C-M/Au.
To further verify the properties of the Ta2C-M modified structure, the
TEM experiment was performed. (see Fig. 4(a)) The thickness of the
Ta2C-M layer is close to 2.35 nm, which is shown in detail in the
embedded image. In Fig. 4(b), an HRTEM image of a thin Ta2C-M layer
with many nanoscale holes in the {1010} plane is depicted along with
the {0001} axis, which indicates the MXene coating is still in the

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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 3. (a) Diagram of the Ta2C-M/Au/TFBG sensor. (b) SEM cross-sectional image of Au/TFBG sensor. (c)-(f) show the morphological distribution of Ta2C-M on Au/
TFBG sensors for different deposition times (50–200 min); the inset map further indicates the growth state of Ta2C-M. (g) EDS spectrum of the Ta2C-M/Au/TFBG
sensor (150 min) with the Ta, C, Au, O elemental mapping analysis (hI -hⅣ ). (i) Real-time offset of the CP2 with the deposition of Ta2C.

crystalline state. The hexagonal structure of the Ta2C-M layer can be
identified. In the {1010} plane, the planar spacing of Ta-Ta and Ta-C are
2.8 Å and 2.6 Å, respectively, which is closer to the study of [36].
Furthermore, in Fig. 4(c), the SAED pattern in the Ta2C-M {0001} axis
describes {1010} diffraction and well-developed {0110}, {1120}
planes, which verifies the presence of the MAX phase in the
photo-deposited Ta2C-M film. The inset shows the HRTEM region along
the {0001} axial direction obtained from the SAED experiment [37].
Subsequently, the elemental composition and chemical state of the
Ta2C-M/Au structure were deeply analyzed by XPS spectroscopy. In
Fig. 4(d), the XPS survey spectrum of the composite structure is depic­
ted, Au and Ta elements are present in the spectrum except for C 1 s
(285.0 eV) and O 1 s (532.5 eV). The high-resolution spectra of the Au
4 f and Ta 4 f regions of the Ta2C-M/Au structure are shown in Fig. 4(e),
(f), respectively. In Fig. 4(e), the two peaks of Au 4f5/2 and Au 4f7/2 at
87.61 eV and 83.95 eV support the introduction of crystalline Au [38].
In Fig. 4(f), the high-resolution XPS scan of Ta 4 f found a dominant
characteristic peak in the V oxidation.
state of Ta5+ at 26.07 eV, and a relatively obvious characteristic peak
IV oxidation state Ta4+ at 23.43 eV exists. In addition to the 4 f peak at
22.42 eV, there are two characteristic peaks at 24.54 eV and 28.09 eV
produced by the TaCx f 5/2 and TaCx Oy 4f 5/2 orbitals, respectively
[39]. This verifies the presence of oxygen-containing groups in the
deposited Ta2C film.
Moreover, the Raman scattering spectrum of the Ta2C-M/Au/TFBG
sensor surface is shown in Fig. 4(g). The Ta2C-M-modified Au structures
exhibit representative characteristic peaks around 237.58 cm-1,
650.54 cm-1, and 1577.59 cm-1 attributed to the vibrational response of
Ta-O, Ta-C, and C-C covalent bonds, respectively [40]. Moreover, the
inset of Fig. 4(g) shows the Raman mapping of 20 × 20 µm2 from the
Ta2C-M/Au/TFBG sensor, corresponding to the characteristic peak at
1577.59 cm-1. Uniform color blocks indicate the uniformity of the
Ta2C-M film, which avoids differences in proton polarization response
due to uneven axial coverage. In addition, surface water droplet contacts
angle test pairs of Au/TFBG and Ta2C-M/Au/TFBG are shown in Fig. 4
(h), (i). The water contact angle of the sensor decreases from 90◦ to 45◦
due to the unique structure of Ta2C-M and the modification effect
brought about by the oxygen-containing groups. The surface modifica­
tion of the sensor can significantly promote the contact area and
adsorption of the sensor surface to the detected molecules, which is an
excellent advantage in the detection of trace molecules. In brief, the
above features demonstrate the success of the Ta2C-M/Au/TFBG
sensor-loaded hybrid structure, which can be used for the following SPR
detection.

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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 4. (a) TEM image of Ta2C-M/Au structure. (b) HRTEM of a prismatic {1010} plane decorated with Ta2C-M along the {0001} axis on Au film. (c) The SAED
pattern of Ta2C-M has characteristic diffraction of {1010} and developed hexagonal Max phases of {0110}, {1120}, the inset shows the HRTEM along with the
{0001} axis. XPS spectra in (d) survey, (e) Au 4 f and (f) Ta 4 f regions of Ta2C/Au structure. (g) SERS spectra of Ta2C and the inset shows the SERS mapping of the
1577.59 cm-1 peak. (h) and (i) Surface water droplet contact angle tests are shown for Au/TFBG and Ta2C-M/Au/TFBG structures, respectively.

3.3. Performance testing of Ta2C-M/Au/TFBG sensors with different
parameters
To explore the performance of the Ta2C-M/Au/TFBG sensor, the
polarization signal responses were further analyzed (see Fig. 5(a) for the
detection schematic diagram). Fig. 5(b) shows the comparison of the
amplified spectra of Ta2C/Au/TFBG and Au/TFBG sensors in 1.3600
ethanol solution, where the position of the SPR signal is shifted toward
the long band (about 1.18 nm). Comparison of the SPR spectra of CP2
collected from Ta2C-M/Au/TFBG sensors (growth conditions:
50–200 min) in ethanol solutions with RI of 1.3600–1.3604 shows that
the minimum of the curve becomes red-shifted (See Fig. 5(c)-(f)), which
verifies the influence of SPPs brought by the SEM morphology changes
corresponding to Fig. 3(c)-(f). In particular, the inset of Fig. 5(f) shows
that the attenuation of the SPR signal becomes blurred and the detection
performance drops sharply, indicating that the overloaded Ta2C-M in­
terferes with the coupling of the internal modulation of the grating with
the high-loss SPW. The sensitivity and FOM of Ta2C-M under different
deposition conditions were statistically presented in Fig. 5(g). The
optimal sensitivity (232.75 nm/RIU) was obtained under the photo-
deposition condition of 150 min, which verified that the introduction
of Ta2C-M material increased the sensor’s detection performance and
signal resolution. Moreover, the excellent linear response relationship
(0.99903) and FOM’s enhancement in Fig. 5(h) demonstrate this con­
dition’s superiority. In addition, reproducibility is another critical factor
that limits the application of laboratory equipment. The spectra of six
different Ta2C-M/Au/TFBG sensors were collected in 1.3600 ethanol
solution, as shown in Fig. 5(i). The good detection performance and
reproducibility indicated that the Ta2C-M/Au/TFBG sensor could serve
as an excellent molecular detection platform.
3.4. Sensitization mechanism and simulation verification of Ta2C-M
The sensitization mechanism of Ta2C can be analyzed by energy
band theory. The enhancement mechanism of Ta2C-M is shown sche­
matically in Fig. 6(a). Under laser irradiation at appropriate

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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 5. (a) Regional schematic diagram of Ta2C/Au/TFBG sensor for ethanol detection. (b) Spectral close-up of Au/TFBG and Ta2C-M/Au/TFBG sensors (150 min) in
1.3600 ethanol solution. (c)-(f) show the CP2 transmission signal response of the Ta2C-M/Au/TFBG sensor (growth conditions: 50, 100, 150 and 200 min)
in1.3600–1.3604 ethanol solutions. The inset in Fig. (f) shows a close-up view of the SPR transmission signal. (g) and (h) are the sensitivity, FOM and linearity of the
CP2 for different growth conditions of Ta2C, respectively. (i) Spectrogram collected from six various Ta2C-M /Au/TFBG sensors in 1.3600 medium.

wavelengths, free electrons are excited from the unoccupied orbitals of
the Au Fermi energy level to jump to holes in the affinity energy level of
the Ta2C-M layer and generate transient negative ions. Subsequently,
the relaxation instant electrons return to the spots below the Au Fermi
energy level, which forms the fundamental part of the exciting radiation
increasing the effective refractive index and substantially amplifying the
polarization efficiency of the system [27]. The introduction of Ta2C-M
reduces the energy required for electron transfer at the Fermi energy
level due to the blocking of the interband transition. In addition, the
effective refractive index of Ta2C-M films is sensitive to the change in
chemical potential (μc ). The relationship between the conductivity (σ )
and μc of Ta2C-M can be expressed as the following equation [41]:
[ ]
e2 k T μc ( ) e2 2|μ | − (ω + i2τ)ћ
σ=i 2 B + 2ln e− (μc /kB T) + 1 + i ln[ c
πћ (ω − j2τ) kB T 4πћ 2|μc | + (ω + i2τ)ћ
where e is the electron’s charge, kB is the Boltzmann taper, T and τ are
the ambient temperature and vibrational frequency, and ћ is Planck’s
constant. The high adsorption of the Ta2C-M material can cause slight
swelling by fusing with the water molecules of the detection solution,
leading to an increase in the interaction space with Au. The effective
refractive index perturbation between the Ta2C-M film and the fiber
cladding will become smaller simultaneously, which leads to a decrease
in the imaginary part of the effective refractive index. Therefore, the
power reflectivity exhibits a decrease, manifested as a decrease in the
amplitude of the cladding resonant mode. Further, the bulk phase en­
ergy band of Ta2C-M was obtained based on VASP, as shown in Fig. 6(b).
The dotted line marked in the red area is the Fermi level, and the mul­
tiple red marked points indicate that the Ta2C-M film in the bulk phase
behaves as a metallic phase. This reflects different characteristics from
other 2D materials and will introduce more robust carrier migration
efficiency to improve the sensor’s detection performance and analysis
] capabilities. The insets ① and ② represent the Ta2C-M coatings in
natural and momentum spaces, respectively. ① Indicates that the Ta2C
(4) layer is a multilayer film structure (refer to TEM). ② shows the high
symmetry point of the Brillouin zone of the Ta2C-M film (marked in red)
and the Brillouin zone of the energy band HEX lattice (path: Γ-M-K-Γ-A-
L-H-A).
Subsequently, the sensitization performance of the Ta2C-M film for

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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 6. (a) Schematic diagram of Ta2C-M’s operation mechanism. (b) shows the energy band diagram of Ta2C-M material obtained by VASP. (The calculated pa­
rameters see Fig. S2) (c) and (d) The electric field distribution on Au and Ta2C-M/Au surface obtained by the difference method based on COMSOL. (e) and (f)
COMSOL-obtained 2D variation plots of the SPR response fit for Au/FBG and Ta2C-M/Au/FBG sensors.

TFBG sensors was further analyzed based on COMSOL. The surface SPPs
responses of Au and Ta2C-M/Au structures were obtained based on the
differential method, as shown in Fig. 6(c), (d). In Fig. 6(c), the apparent
uniform fringe spot on the Z-axis indicates the plasmon resonance
coupling effect of the multimode tilted grating on the coating surface. In
Fig. 6(d), the more substantial electromagnetic distribution and electric
field amplitude indicate the enhancement of Ta2C-M. Furthermore, the
fitting evaluation of the SPR behavior of the two sensors, Au/FBG and
Ta2C-M/Au/FBG, refers to the experimental medium in the RI envi­
ronment of 1.3600–1.3605 (see Fig. 6(e) and (f)). Compared to the Au/
TFBG sensor, the Ta2C-M/Au/TFBG sensor exhibited a stronger fitted
SPR behavior (235 nm/RIU) showed a high agreement with the exper­
iment. And the fitted loading redshift (~0.95 nm) of the Ta2C-M coating
is similar to the experimental data. Moreover, the obvious FOM
improvement is also reflected in the width variation of the wavelength-
shifted patches. The enhancement of the electric field amplitude and the
optimization of the SPR fit evaluation reflect the sensitizing effect of the
Ta2C-M material.
3.5. Application detection of Ta2C-M/Au/TFBG sensor
To further demonstrate the applicability of the proposed Ta2C/Au/
TFBG sensor, we performed a comprehensive evaluation of two mole­
cules with carcinogenic risk, saccharin and BHT, respectively. The
schematic diagram of Ta2C-M/Au/TFBG sensing area for SPR and SERS
detection is shown in Fig. 7(a). Molecules of two common cancer species

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W. Yang et al. Sensors and Actuators: B. Chemical 369 (2022) 132391

Fig. 7. (a) Schematic representation of the molecular assay. (b) SERS spectra of saccharin and BHT molecules (The relevant homogeneity and repeatability tests are
shown in Fig. S3). SPR spectra were obtained using Ta2C-M/Au/TFBG sensors under 10-12-10-3 M saccharin (c) and BHT (d). (e) and (f) show the amplitude and
wavelength variation statistics of the Ta2C/Au/TFBG sensor in different saccharin and BHT environments.

can be effectively captured based on the high adsorption of Ta2C-M
oxygen-containing groups, which can be used for SERS qualitative
analysis of the molecules while realizing the evaluation of SPR behavior.
The high-resolution spectrum at 10-4 M concentration provides stable
resolving power in practical detection, and the characteristic peaks of
Saccharin and BHT are similar to [42] and [43], respectively. Subse­
quently, the multi-gradient detection of two media, Saccharin and BHT,
with solution concentrations of 10-12-10-3 M, were collected by the
Ta2C/Au/TFBG sensor as shown in Fig. 7(c) and (d), respectively. A
similar detection trend is collected: the amplitude change of the trans­
mission spectrum gradually decays with decreasing concentration, as
shown in Fig. 7(e). In addition, the Ta2C/Au/TFBG sensor shows a
standard linear trend of 0.98524 and 0.98919, respectively, corre­
sponding to a range of 10-8-10-3 M for both Saccharin and BHT mole­
cules, as shown in Fig. 7(f). However, the SPR behavior shows a
saturation line response with different curvatures as the detection
concentration decreases, verifying that the sensor has a resolution limit
of 10-11 M for molecules. Therefore, the proposed Ta2C/Au/TFBG sensor
has perfect SPR resolution and excellent application prospects.
4. Conclusion
An ultra-sensitive Ta2C-M/Au/TFBG SPR sensor was proposed and
investigated based on the beneficial sensitization of Ta2C-M. Under
optimal laser-induced conditions for 150 min, we achieved SPR
spectroscopy-based ethanol detection and trace analysis of two carci­
nogenic risk molecules, saccharin and BHT. The energy band theory of
the Ta2C-M coating was calculated to explain the sensitization mecha­
nism of its SPPs based on VASP. And based on the 3D simulation model
of TFBG proposed by COMSOL, the electric field gain brought by the
introduction of Ta2C-M was analyzed to fit the SPR detection perfor­
mance of the two sensors. In addition, the multi-coupling modes, the

9
W. Yang et al.
polarization of the sensitive layer, the transmission mode, and the
electromagnetic distribution of the TFBG sensor were systematically
analyzed. Therefore, we believe that the Ta2C-M/Au/TFBG SPR sensor
will provide a promising approach to biochemical analysis and micro-
quantification evaluation.
CRediT authorship contribution statement
Wen Yang: Conceptualization, Methodology, Software, Experiment,
Writing – original draft, Writing – review & editing. Yangyang Cheng:
Conceptualization, Methodology, Software. Runcheng Liu: Experi­
ment, Writing – original draft.
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.
Acknowledgments
The authors are grateful for financial support from the National
Natural Science Foundation of China (62073193, 81972007,
12074226).
Appendix A. Supporting information
Supplementary data associated with this article can be found in the
online version at doi:10.1016/j.snb.2022.132391.
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Wen Yang is a doctoral candidate at Shandong University. He studies the preparation and
physical property characterization of metamaterials, and the preparation and application
of tilted grating fiber SPR biosensors.
Yangyang Cheng is a doctoral candidate at Shandong University. His main research is
damage detection and fatigue life prediction, and he is good at COMSOL, Abaqus and other
simulation software.
Mingshun Jiang is a professor at Shandong University. His main research areas are smart
sensors, structural health inspection, fault diagnosis, digital twin and visualization, and big
data analytics. He has led 2 National Natural Science Foundation of China, 1 National Key
R&D project, 5 military research projects, and 3 provincial and ministerial level research
projects. Cumulative research project funding reached more than 30 million RMB. He has
published more than 40 papers as the first author or corresponding author, including more
than 30 SCI-indexed papers. He has applied for 12 patents as the first inventor, and has
been granted 6 invention patents and 8 software copyrights.
11
Sensors and Actuators: B. Chemical 369 (2022) 132391
Shouzhen Jiang is a professor at Shandong Normal University. His research interests
include: 1) 2D materials and metal nanoarray preparation, 2) ultrafast mode-locking field
of lasers, 3) surface plasmon resonance sensor field, and 4) Raman-enhanced substrate
field. He has published more than 90 papers related to it and applied for more than 10
patents.
Runcheng Liu is currently enrolled in a Master’ degree at Shandong Normal University,
China. His research interests are focused on surface plasmonic photonics and surface-
enhanced spectroscopy.
Jiajun Lu is a doctoral candidate at Shandong Normal University. He studies valleytronics
materials’ design and electronic properties by performing first-principles and ab initio-
based tight-binding approach.
Lutao Du, M.D., Ph.D., is currently professor of Shandong University. He was awarded the
Youth Committee of Chinese Society of Laboratory Medicine in 2018 and the young ex­
perts of Taishan Scholars in 2019. His research interests mainly focus on tumor marker for
early diagnosis and plasmonic nanostructures for spectroscopy technology. He is also
committed to exploring nano-diagnostics of marker detection. In recent years, he has
undertaken 8 scientific research projects including the Natural Science Foundation of
China and the Key Research and Development Program of Shandong Province. His
research efforts have been published in excess of 50 scientific papers and issued 8 national
patents.
Peilong Li is a professor works at The Second Hospital, Cheeloo College of Medicine,
Shandong University. He has been committed to the basic and clinical application research
of the drug resistance mechanism and predictive markers of tumors. As the project leader,
he has received the National Natural Science Foundation of China and Shandong Natural
Science Foundation. In the past five years, as the first author or corresponding author
published 7 SCI-indexed papers and one paper was awarded ESI TOP1% high-cited paper
with 142 citations.
Chuanxin Wang, M.D., Ph.D., is a professor of Shandong University and president of The
Second Hospital of Shandong University. He also is currently the chair-elect of Chinese
Society of Laboratory Medicine, vice chair of Chinese Medical Doctor Association of
Laboratory Medicine, etc. His recent research interests mainly focus on tumor exosomal
markers and new detection technology, especially the intersection of nanotechnology and
biomedicine. In recent years, he has undertaken 12 scientific research projects including
National Key Research and Development Project and the projects of Natural Science
Foundation of China. More than 100 SCI articles were published in recognized journals and
15 national patents were issued.