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. 2026 Feb 4;11(6):9734–9741. doi: 10.1021/acsomega.5c10195

Synthesis and Fabrication of MXene/MWCNT Nanocomposites for Electronic Detection of Sulfamethoxazole

Seyadu Abuthahir P §, Manikandan E †,‡,*
PMCID: PMC12917796  PMID: 41726711

Abstract

The significant demand for accurate and accessible sensors has led to significant advances in nanotechnology. This is especially relevant to the use of advanced nanomaterials; in this study, a hybrid composite of MWCNTs and MXene was produced. The MXene/MWCNT composite was made by sonication procedures and subsequently assessed by using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) to verify successful integration and enhanced structural properties. The produced sensor exhibited a detection limit of 3.053 μg/L and a sensitivity of 2.55 mA μg–1 L. Additionally, it demonstrated exceptional electrical performance and a linear, beneficial response to varying SMX concentrations. This potential of MWCNTs/MXene-based sensors makes them effective tools for detecting pharmaceutical residues with high sensitivity for practical field uses.

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1. Introduction

The development in biosensing creates a need for accurate, sensitive, and reliable sensors, which has ignited rapid and innovative advancements in nanotechnology. Numerous nanomaterials, including graphene, carbon nanotubes, metal nanoparticles, and quantum dots, have been at the cutting edge of this progress. These materials are well suited for sensor design because of their special physicochemical properties, which substantially enhance sensitivity, selectivity, and response time in a range of application areas, such as environmental monitoring, clinical diagnostics, and food safety. , Multiwalled carbon nanotubes (MWCNTs) have attracted particular importance as they hold promise as a biosensing technology. Their excellent structural and functional properties such as high electrical conductivity, remarkable mechanical strength, chemical stability, and large surface-to-volume ratio allow for the optimal immobilization of biomolecules and the transduction of biological signals. These qualities are important for the detection of target analytes present at ultralow concentrations, making MWCNTs an efficient tool in the development of next-generation sensors designed for early illness diagnosis, pollutant detection, and food contamination evaluation. ,

MWCNTs hold an outstanding characteristic that makes them a suitable fit for sensors based on chemi-resistive sensors, which have a tendency to detect analytes with high sensitivity, in real time, and in a label-free manner. Employing the electrical properties of MWCNTs, the field effect transistor’s chemi-resistive sensor-based design senses changes in charge distribution when biomolecules such as glucose, antibiotics, or other tiny molecules adhere to the sensor surface. , Chemi-resistive sensors are the ideal, affordable technology for real-time biosensing applications. They can convert these changes into very sensitive electrical signals. The detection of several biomarkers, like glucose and antibiotic residues, has been a very common application for MWCNT-based chemi-resistive sensors, proving their use in healthcare monitoring. Researchers are interested in emerging nanomaterials like MXenes to further enhance the performance of MWCNTs. The MXene family of two-dimensional (2D) materials, which consists of transition metal carbides, nitrides, or carbonitrides, possesses perfect hydrophilicity, tunable surface chemistry, and electrical conductivity. , on improving the overall sensitivity of the sensor devices. Hence, MWCNTs and MXene work together to solve sensitivity and homogeneity. When added to MWCNT-based sensors, the surface of MXene becomes more active; also, the charge transfer and overall sensor performance are enhanced across a range of environmental applications.

Composites of MWCNTs and MXenes show great potential for the detection of antibiotics like sulfamethoxazole (SMX), which is a significant contributor to environmental contamination. Most of the water sources are frequently contaminated by SMX, which is one of the major antibiotics that are widely used in both human and veterinary medicine, as a result of its widespread use and inadequate wastewater treatment systems. The clean and contaminant-free environment and human health are the major reasons to be addressed through the overcoming of widespread pollution, which also plays a role in the development of antibiotic resistance. The ability to identify SMX at low concentrations in water is important to maintaining water quality and preventing additional damage to the environment. , Traditional methods such as spectrometry and chromatography are commonly used to detect SMX; however, they are complicated for field usage, require sophisticated equipment, and are also time-consuming processes. However, MX/MWCNT composite-integrated chemi-resistive sensors offer a compact, cost-effective, and rapid alternative to onsite testing. These sensors utilize the large surface area of MWCNTs and the superconductivity of MXenes to detect SMX at low concentrations by observing electrical changes and to evolve a real-time alternative for water quality monitoring in industrial and remote locations. , By lowering interference from other ambient chemicals, which is a major problem when considering complicated real-world samples, the incorporation of these composite materials into sensors further improves the sensitivity for SMX. To detect SMX, traditional methods such as spectrometry and chromatography are commonly used; however, they are not the most effective for field use, are time-consuming, and need sophisticated equipment. Contrarily, MX/MWCNT composite-integrated chemi-resistive sensor-based sensors offer a rapid, reasonably priced, and transportable alternative to on-site testing. By employing the large surface area of MWCNTs and the high conductivity of MXenes to identify SMX at extremely low concentrations by recording electrical changes, these sensors provide a real-time alternative for water quality monitoring in both industrial and remote situations. , By decreasing interference from other ambient chemicals, which is a major problem in complicated real-world samples, the incorporation of these hybrid materials into chemi-resistive sensors further improves the sensor’s selectivity for SMX.

Furthermore, the sensitivity of the sensor for SMX can be altered by functionalizing MXene surfaces, which enhances its ability to detect the antibiotic in complex aqueous matrices. This development in sensitive, scalable, and real-time monitoring systems is crucial due to the global problem of antibiotic contamination in water. FET-based sensors using MX/MWCNT composites exhibit remarkable sensitivity and selectivity that exhibit the same level of chemi-resistivity and can identify a variety of environmental contaminants, such as antibiotics, pesticides, heavy metals, and pharmaceuticals. When considering Internet of Things (IoT) systems, all these sensors have the potential to upgrade environmental monitoring by providing continuous, real-time data that may direct prompt and respective actions to address water contamination. This study builds on previous findings demonstrating the revolutionary potential of hybrid nanomaterials in biosensing applications. By synthesizing MX/MWCNT composites and incorporating them into chemi-resistive sensor designs, we developed a sensor that can identify SMX in water samples with sensitivity. The primary goals of the study are to develop a chemiresistive sensor, to synthesize and characterize the composite material, and to evaluate the sensor’s capacity to detect the different SMX concentrations. This work aims to contribute to the development of advanced analysis tools for both healthcare and environmental monitoring.

2. Material Synthesis and Fabrication Method

2.1. MXene Synthesis

The MXene was prepared by an etching technique that involves etching of Ti3AlC2 powder (Ultra nanotech, 99.5%) with 40% hydrofluoric acid (HF) for 24 h at room temperature. Deionized water was used to completely wash the mixture until the pH was neutral after etching. Further, the material was washed and centrifuged with deionized water and ethanol. The resultant sample was dried in a vacuum oven at 60 °C. When X-ray diffraction (XRD) revealed the distinctive peaks of the Ti3C2 phase, it was proven that the MXene had successfully formed. ,

2.2. MX/MWCNT Composite Preparation

The synthesis procedure of MX/MWCNTs was initiated by separately dispersed in deionized water using bath sonication for 30 min in order to create the composite. This first stage ensured that the two components were thoroughly separated before mixing and assisted in dissolving any agglomerates. Following their individual dispersions, the two substances were combined in a 1:1 molar ratio. The precursor ratio (1:1, MXene: MWCNTs) in this investigation was taken straight from a work that claimed this ratio was useful for fabricating stable MXene/MWCNTs hybrid films with high dispersion and conductivity. We adhered to the literature-recommended ratio without making any additional adjustments because our goal was to assess the composite’s sensing capabilities rather than optimize the ratio. We recognize that systematic optimization might enhance performance; however, this was outside the scope of our study. In line with the cited paper, the selected 1:1 ratio resulted in reproducible films and steady electrical activity in our apparatus. In the updated text, we now explain this reasoning and include a citation to the relevant publication. To get a uniform dispersion, the mixed suspension was subsequently put through 120 min of tip sonication. In order to maintain the temperature constant and prevent any heat-induced degradation of the nanomaterials, an ice bath was maintained throughout the sonication procedure. The MXene flakes and MWCNTs were able to fully interact over this extended sonication period, producing a stable and evenly distributed composite. To eliminate any excess solvent, the mixture was dried in a vacuum oven.

2.3. Electrode Fabrication

The MXene/MWCNT composite was weighed at 5 mg and dispersed with 1 mL of ethanol. This was followed by pipetting 10 μL of this dispersion on the PET substrate and spinning it at 3000 rpm for 60 s. Ten repetitions of this 10 μL deposition step produced a continuous, homogeneous sensor coating with sufficient thickness and conductivity. The PET substrates were cleaned by sonication in isopropyl alcohol. The PET substrates were then spin-coated with the MX/MWCNT composite for 60 s at 3000 rpm. The device was annealed in a hot plate for 2 h at 60 °C to increase the composite film’s conductivity and stability. Lastly, source and drain electrodes were made on either side of the substrate using copper tape. , The entire experiment is illustrated in Scheme .

1. Schematic Representation of the Overall Workflow: Synthesis of the MXene/MWCNT Composite, Fabrication on the PET Substrate, and Sensing Techniques.

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3. Structural and Morphological Characterization

3.1. XRD

The crystalline structure of the MX/MWCNTs was investigated by using X-ray diffraction (XRD), as seen in Figure . The clear emergence of the MWCNTs’ characteristic diffraction peaks at 2θ = 25.8°, 42.9°, and 53.4° Figure S2. The integration of MWCNTs into the MXene framework confirmed their successful incorporation into the composite structure. The XRD pattern in Figure S1 confirms the synthesized MXene. Etching of the MAX phase (Ti3C2T x) is confirmed by the complete disappearance of the diffraction peak 2θ = 38.8°, which corresponds to the (104) plane, indicating the removal of the Al layer. The (002) and (006) planes represent the layers of the MXene at 8.7° and 18°, respectively. The MWCNTs’ XRD pattern shown in Figure S2 presents a sharp diffraction peak at 26° assigned to the (002) plane of graphitic carbon. It indicates the interlayer spacing of graphitic structure, which confirms the crystallinity of carbon nanotubes. A weak shoulder or broad hump at higher angles (40–45°) corresponds to the (100)/ (101) graphitic planes, consistent with typical multiwalled nanotube structures. These features confirm that the MWCNTs retain their graphitic ordering and are suitable as conductive pathways for composite formation.

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XRD pattern of MX/MWCNTs.

Notably, the MXene peaks in the MX/MWCNT composite are located at 2θ = 18.6° and 27.8°. These peaks slightly shift; this indicates that MWCNTs were effective in intercalating between the MXene layers, causing the interlayer gap to significantly widen. By expanding the surface area and number of sites available for electrochemical interactions, this structural alteration enhances the material’s potential for sensor applications. These XRD results in Figure demonstrate the effective formation of the MX/MWCNT composite, which added MWCNTs to improve conductivity and sensitive stability while preserving the structural integrity of MXenes.

Raman spectroscopy is carried out to characterize the MX/MWCNTs, which provides the material purity state. In Figure , the peaks observed at 154.5 cm–1, 200.8 cm–1, and 204.2 cm–1 are attributed to Ti–C bonding vibrational modes. 403.2 cm–1 corresponds to the deformation of the Ti–C bond and can originate as an in-plane C vibration and Ti–C bond distortion. Surface oxidation is also observed at 507.3 cm–1 and 623 cm–1. These indicate the possibilities in the formation of TiO2 by the surface exposure in the atmosphere of the synthesized MXene sample. The disorder of the carbon structure with respect to MWCNTs is established at 1349.6 cm–1 (D band), and also, the vibrational mode of MWCNTs arising at 1566.5 cm–1 (G band) reveals the in-plane stretching of sp2 carbon atoms with the disorders. The defect quality of the synthesized material is analyzed by the D/G intensity ratio, eq , I D/I G, for D and G band intensity values

IDiG=24642657=0.93 1

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Raman spectrum of MX/MWCNTs.

The ratio indicates a moderate disorder in the MWCNT structure upon functionalization with the MXene.

I2DiG=2640.82657=1 2

The second-order peak at 2677.5 cm–1, with respect to the 2D band, is recorded, and the calculated ratio, eq , of the 2D/G band is 1, which is associated with the multilayer presence of MWCNTs.

3.2. FESEM

The synthesized MX/MWCNTs composite’s surface morphology was examined with FESEM. The resulting FESEM pictures were taken at 200 and 400 nm magnifications. The area indicated in Figure a demonstrates that MWCNTs are uniformly distributed throughout the MXene sheets’ surface, same as the sheet representation of the MXene, Figure S4, a multilayered sheet of well lamellar structure. These layers represent the etching of the MAX phase, forming thin flakes with large dimensions. The FESEM image of MWCNTs in Figure S5 displays a dense arrangement of long, tubular nanotubes with rough outer walls. The nanotubes in the image show uniform formation in an interconnected framework. Their high aspect ratio and entangled structure support effective electron transport when incorporated into composite materials. Figure b also shows the exact shape of the MWCNTs, recorded on a scale of 200 nm. The average diameter of the nanotubes is measured to be 41 nm. The nanotubes’ average diameter was found to be approximately 41 nm. MWCNTs seated on the MXene sheets in images are clearly visible, and the consistent morphological features demonstrate that the MX/MWCNT composite was successfully synthesized and produced.

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FESEM images of MX/MWCNTs: (a) 400 nm and (b) 200 nm.

The TEM micrograph of the MXene/MWCNTs composite in Figure presents the characteristic combination of thin MXene nanosheets and MWCNTs in a hybrid network. The blue arrow marked in the image is MXene flakes that appear semitransparent, layered with irregular lateral dimensions, while the MWCNTs are observed as long, hollow tubular structures intertwined throughout the layered MXene sheet. The nanotubes are distributed on the entire MXene sheet, indicating good physical contact and interfacial coexistence. The MXene provides anchoring sites and enhances the dispersion of the nanotubes. This resulting interconnected architecture supports enhancing electron-transport pathways and increasing accessible surface area for analyte interaction.

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TEM image of the MXene/MWCNTs.

The investigation of XPS was to understand the surface chemical nature of the MXene/MWCNT elements and chemical bonds. Figure a shows the characteristic peaks at 285, 457, 532, and 683 eV that correspond to C 1s, Ti 2p, O 1s, and F 1s, respectively. Figure b shows the Ti 2p spectrum, which is located at 456.5 and 462.2 eV due to the presence of Ti–C–O, CO, and adsorbed water in Figure c,d. , The C–C and C–N peaks at 284.8 and 285.8 eV, respectively, show the C 1s spectrum in 3d. T-F is represented by the high-resolution F 1s spectrum in Figure e.

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XPS spectra of MX/MW: (a) survey, (b) Ti 2p, (c) O 1s, (d) C 1s, and (e) F 1s.

4. I–V Analysis

The electrical performance of the sensor was characterized by current–voltage (I–V) measurements, which were performed by a two-probe setup system in a Keithley 2450 EC system. The adopted two-probe chemi-resistive configuration for detecting SMX was motivated by its compatibility with flexible substrates and proven effectiveness in nanomaterial-based chemical sensing. Chemi-resistive devices operate on the principle that analyte interaction directly modulates the electrical resistance of the sensing film, enabling label-free and low-power detection without the need for external gate modulation or dielectric engineering. Such two-terminal architectures are widely used for MXene, MWCNT, and carbon-based sensors because they allow direct measurement of charge-transfer and adsorption-induced conductivity changes across the channel. Compared to field-effect transistors (FETs), which require a well-defined gate electrode, the dielectric layer. Moreover, chemi-resistive architectures offer advantages in scalability, mechanical flexibility, low fabrication cost, and rapid prototyping, making them an attractive option for screening material performance and developing early-stage sensing platforms. The source and drain electrodes are connected to the system and measured via I–V analysis. The tests are demonstrated to measure the electrical conductivity and stability of the composite material device; these are essential for evaluating the consistency of sensor performance.

4.1. Sensing of MX/MWCNTs

The sensor showed an efficient and consistent response to varying concentrations of SMX. MWCNTs are excellent electrochemical platforms for electrochemical sensing electrodes; we selected MXenes to form the composite because of the synergistic morphology and interfacial engineering. The lamellar MXene sheets with the entangled MWCNT network form highly porous and interconnected structures. This structure increases the effective electroactive area by exposing more MXene lamellae for SMX adsorption, as the MWCNTs are physically over the sheets. The MXene, in turn, improves the electronic coupling of MWCNTs, creating continuous electron-transport pathways throughout the hybrid for sensing. This conductive and porous framework, directly supported by the observed SEM morphology, enhances rapid charge transfer, improves electrolyte penetration due to the MXene’s hydrophilicity, and overcomes the hydrophobic limitations of pristine MWCNTs. The structural features visible in the SEM image justify the integration of the MXene with MWCNTs and explain the improved sensing performance toward SMX.

The measured current decreased as the SMX level increased, indicating an inverse dependence and validating the ability of the sensor to reliably and sensitively detect analytes. The interaction between the SMX molecules and the MX/MWCNT composite, which explicitly emphasized the enhancement of charge transfer at the sensor interface, dropped the current to 0.010 A at larger SMX concentrations of 24 μg. The initial attempts to analyze the sensor response over a larger concentration range of SMX indicated that response saturation was above 24 μL of the analyte, which corresponds to the highest concentration limit employed in this experiment. At larger concentrations, the current response saturated and showed no difference with the current. The MXene/MWCNT composite’s surface site saturation, in which too much SMX adsorption fills or blocks the active interaction sites and stops further channel resistance modulation. Therefore, reliable calibration curves requiring a strictly linear concentration over this upper limit were excluded from the LOD. The sensor performs best in the linear region below 24 μL. The I–V responses of the composite are improved from the base MXene. The I–V characteristics were evaluated on PET substrates under similar circumstances. During the applied voltage sweep, the MXene-only film displayed a very low current output, between 1.0 × 10–5 and 4.0 × 10–5 A, which is over 200 times lower than the composite device shown in Figure S3. Because of the substantial sheet restacking and restricted electron-transport routes indicated by this poor conductivity, the MXene by itself is not appropriate for sensitive SMX detection. This is increased because of the interaction between the analyte and the MX/MWCNTs, suggesting increased resistance. At lower concentrations, 5–10 μg, the current was higher, 0.016 A, indicating less resistance where there were fewer SMX molecules interacting with the composite.

4.2. Detection of SMX and Sensor Performance

I–V measurements were used to analyze the performance of the MX/MWCNT-based sensor over a current limit of 0.1 A within the voltage range of 0–2 V, as presented in Figure a. The sensor demonstrated a strong linear connection between 4 and 24 μg/L and was able to detect SMX concentrations clearly and consistently. The current density increases linearly with voltage for all concentrations, indicating ohmic behavior and stable electrical contact between the electrode and the composite, Figure b. The sensing capability of the composite was determined using the relative resistance change (ΔR/R 0), as shown in Figure c. A significant rise in ΔR/R 0 with an increasing SMX concentration, particularly above 10–12 μg, indicates strong modulation of the device resistance at higher analyte levels. At lower concentrations (4–8 μg), the limited adsorption on accessible active sites causes minimal resistance changes. ΔR/R 0 increases significantly at higher concentrations, suggesting better charge-transfer interactions between SMX molecules and MXene/MWCNT hybrid channels, as well as surface site saturation. This quantitative and accuracy of detection capabilities of the device were confirmed with a correlation coefficient (R 2) of 0.956 from Figure . As the SMX concentration on analysis, molecule adsorption onto the composite surface and reflect with lower charge carrier mobility, the output current dropped as the SMX concentration rises. This inverse relationship results from analyte binding, which modifies the surface potential and limits electron transport in the charge channels inside the nanocomposite matrix.

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(a). I–V response of SMX by MX/MWCNTs. (b) Current density analysis of MX/MWCNTs. (c) ΔR/R 0 plot.

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Linear fit response of SMX in MX/MWCNTs.

The standard deviation approach showed a LOD of 3.053 μg/L (0.012 μM), demonstrating better sensitivity and being suitable for detecting SMX trace levels.

Comparison of the performance of our MXene/MWCNTs chemi-resistive sensor with reported nanomaterial-based SMX sensors. Prior studies include CNT electrodes decorated with metallic nanoparticles (e.g., Ag-filled MWCNTs, LOD = 0.01 μM), MXene/MOF (MXene/ZIF-8)-modified GCEs (LOD = 5.1 μM), and graphene/metal-oxide hybrids mentioned in Table . These sensors differ in technique, electrode type, and sample matrix, which affects direct comparison. While nanoparticle-based CNT sensors show very low LODs, our flexible MXene/MWCNT device offers simpler fabrication and good sensitivity with large-area PET substrates. This work’s LOD is higher than that of the best CNT-based systems. This sensitivity is mandatory for applications in public health and environmental surveillance, where identification of low concentrations of antibiotic residues is crucial. The necessity for precise detection methods is highlighted for SMX presence in water bodies and its capacity to spread bacteria resistant to antibiotics. The sensitivity of this device is determined by the current-to-concentration ratio of the difference between each analysis and the maximum voltage reached, which is equal to the LOD requirement. The calculated sensitivity value is 2.55 mA μg–1 L. These sensitivities and LOD are valid for performing sensing devices.

1. Comparison of Existing Nanomaterial-Based Sensors for SMX Detection.

material/electrode sensor type/technique linear range LOD refs
Ag-filled MWCNT composite electrode voltammetric (DPV) 0.05–70 μM 0.01 μM
MXene/ZIF-8-modified GCE voltammetric (SWV) 100–1000 μM 0.153 μM
Graphene/ZnO voltammetric (DPV) 1–40 μM 0.4 μM
MXene/MWCNTs chemi-resistive two-probe (I–V) 1.5–10 μM 0.012 μM this work
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The fabricated sensor response for the concentration ranges of up to 24 μg/L indicated that the active binding sites in the sensing layer were saturated. This pattern is typical of surface-binding sensors and suggests that increasing the surface area or adding functional groups increases the detection range. Nonetheless, the results show how very promising the sensor is for monitoring pharmaceutical contaminants in the real world, offering a rapid, reliable, and reasonably priced method of managing antibiotic contamination and assessing water quality.

5. Conclusion

In conclusion, the synthesis of the composition of MWCNTs and MXene improved the efficacy of I–V analysis-based sensors for SMX detection in water samples. Structural studies revealed that MWCNTs were successfully incorporated into the MXene sheets, increasing the surface area without compromising the stability of the composite. The sensor’s response, strong linearity, sensitivity, and low detection limit over a broad concentration range made it a good choice for environmental monitoring applications. The sensor’s exceptional stability and specificity in detecting SMX residues show that it has the potential to solve the issue of antibiotic contamination in water sources.

Supplementary Material

ao5c10195_si_001.pdf (234.9KB, pdf)

Acknowledgments

The authors thank the Vellore Institute of Technology, Chennai, for providing open-access support.

All data included in the manuscript are available within the article and its Supporting Information.

The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsomega.5c10195.

  • Crystalline properties and FESEM analysis of MXene and MWCNTs and I–V analysis of the pure MXene for SMX sensing (PDF)

S.A.: original draft, materials synthesis, and characterization. M.E.: methodology, supervision, reviewing.

The authors declare no competing financial interest.

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Supplementary Materials

ao5c10195_si_001.pdf (234.9KB, pdf)

Data Availability Statement

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