Raman Spectroscopy Research Articles

Identification of fluoroquinolone-resistant Mycobacterium tuberculosis through high-level data fusion of Raman and laser-induced breakdown spectroscopy.

Accurate and rapid diagnosis of drug susceptibility of Mycobacterium tuberculosis is crucial for the successful treatment of tuberculosis, a persistent global public health threat. To shorten diagnosis times and enhance accuracy, this study introduces a fusion model combining laser-induced breakdown spectroscopy (LIBS) and Raman spectroscopy. This model offers a rapid and accurate method for diagnosing drug-resistance. LIBS and Raman spectroscopy provide complementary information, enabling accurate identification of drug resistance in tuberculosis. Although individual use of LIBS or Raman spectroscopy achieved approximately 90% accuracy in identifying drug resistance, the fusion model significantly improved identification accuracy to 98.3%. Given the fast measurement capabilities of both techniques, this fusion approach is expected to markedly decrease the time required for diagnosis.

Solvent-dependent reaction mechanisms in the electrooxidative coupling of phenols: insights by operando Raman spectroelectrochemistry.

The electrochemical oxidative phenol coupling reaction is a sustainable method for accessing biphenolic compounds. Using the dimerization of sesamol as a model reaction, insights into the reaction mechanism were gained via operando Raman spectroscopy. By varying the solvent and electrodes, different reaction mechanisms were identified and correlated with the respective product yields.

Raman spectroscopy of the ilmenite–geikielite solid solution

Abstract Ilmenite (Fe2+TiO3) and geikielite (MgTiO3) are important terrestrial minerals relevant to the geology of the Earth, the Moon, Mars, and meteorite samples. Raman spectroscopy is a powerful technique that allows for mineral cation determination for the ilmenite–geikielite solid solution. We report on a suite of nine samples within the ilmenite–geikielite solid solution and provide context for their quantitative interpretation. We compare a univariate Raman peak position model for predicting ilmenite composition with a multivariate machine learning model. The univariate model is currently recommended, though the multivariate model may become superior if the data set size is increased. This study lays the groundwork for quantifying Fe (ilmenite) and Mg (geikielite) within oxide minerals using a cheap, portable, and efficient technology like Raman spectroscopy.

Synthesis and physical characterization of novel Ag2S-CdS /Ag /GNP ternary nanocomposite

A new type of Ag2S-CdS/Ag/GNP nanocomposite material was successfully synthesized in the presented work. The structural and physical properties of compounds were studied separately and together. Ag2S-CdS/Ag/GNP nanocomposite materials were studied by Xray diffraction (XRD), Ultraviolet-Visible (UV-Vis), Fourier Transform Infrared (FTIR), Raman spectroscopy and Scanning Electron Microscopy (SEM). Based on the results, Ag nanowires (NWs) were successfully synthesized, and then it was determined that during the hybridization process, two phases of acanthite Ag2S and the cubic crystal system of Ag2O were formed. Then, Ag2S-CdS NWs were formed from mixed monoclinic Ag2S and hexagonal CdS. In the absorption spectrum of Ag NWs, the main absorbance peaks were observed at 357.3 nm and 380.2 nm. The energy gap (Eg) values of the Ag sample are 3.8 eV. The band gap value of Ag2S (2.5, 3.8, 4.6 eV) and Ag2S-CdS (2.5, 3.8, 4.8 eV) have a triple value due to the formation of a hybrid structure. The Raman spectrum of Ag2S-CdS belongs to longitudinal-optical (LO) phonon modes of zinc-blende phase CdS and for the 1, 2, and 3 times spin-coated samples on the surface of GNP/PVA have observed all characteristic Raman peaks, which belong to NWs at 485.13 cm-1, and 960.22 cm-1.

Exploring C3F8 as a gaseous structure H hydrate former: Implications for hydrate-based greenhouse gas separation and recovery

Octafluoropropane (C3F8) is a fluorinated gas (F-gas) known for its high global warming potential. In this study, the role of C3F8 as a novel gaseous structure H (sH) hydrate former was investigated. By employing a comprehensive methodology involving thermodynamic, crystallographic, and spectroscopic analyses, the successful encapsulation of C3F8 into the large cages of sH hydrates was unveiled for the first time. The incorporation of C3F8 into sH hydrates was inferred from a shift in the thermodynamic hydrate phase equilibria, and unequivocal evidence of successful C3F8 encapsulation was obtained using powder X-ray diffraction, 13C nuclear magnetic resonance, and Raman spectroscopy. The findings showed that C3F8 overcame the conventional limitations associated with sH hydrate formers, which are predominantly liquid and solid substances, thereby significantly expanding the scope of potential gaseous sH hydrate formers. This advancement not only enhances the fundamental understanding of gas hydrate formers but also opens up new avenues for hydrate-based technologies, particularly in the separation and recovery of large-size F-gases, which have substantial environmental implications.

Enhancing fiber-reinforced asphalt binders via graphene oxide grafting: A novel interfacial modulation strategy

This study reports a novel interfacial enhancement strategy for fiber-reinforced asphalt binders. The graphene oxide (GO) nanosheets were used and grafted onto polyester (PET) and polyacrylonitrile (PAN) fibers in order to enhance the performance of modified asphalt binders. Prior to this, ultraviolet ozone (UVO) treatment was primarily adopted for activating the inert surface of fibers. Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Scanning electron microscope (SEM) confirmed that GO-modified fibers were successfully prepared via surface modification. For the rheological properties determined by dynamic shear rheometer (DSR), the asphalt binders with GO-modified fibers exhibit improved high-temperature rutting resistance, better creep and recovery characteristics and increased anti-fatigue properties. Remarkably, it demonstrates that the recovery (R) value of GO-PAN modified asphalt binder is increased by 21.9 %, and the non-recoverable compliance (Jnr) value of GO-PET modified asphalt binder has been reduced by 31.9 % compared to that reinforced with the unmodified fiber in multiple stress creep recovery (MSCR) tests. These enhancements are mainly attributed to the increased roughness and modulus of the GO-grafted fibers, which promote effective stress transfer at the fiber-asphalt interfaces. Results from the atomic force microscope (AFM) indicate that the Young’s modulus of GO-PET and GO-PAN is 94.2 % and 260.0 % higher than that of PET and PAN, respectively. This research not only provides a simple and cost-effective method for improving the rheological performance, but also elucidates the enhancement mechanism of interfacial behavior in fiber-reinforced asphalt binders.

Quantitative Raman Spectroscopy of Urea and Thiourea in the Reaction Mixtures of Allantoin and 4,5‐Dihydroxyimidazolidine‐2‐Tione Formation

ABSTRACTThe present work introduces a new approach to quantitative determine the reagent concentrations (thiourea and urea) using in situ Raman spectroscopy in the reaction mixture exemplified by the reactions of formation of allantoin and 4,5‐dihydroxyimidazolidine‐2‐thione. The approach comprises the use of a commercially available immersion probe (MarqMetrix Process Elite BallProbe with sapphire lens) as a standard for the immersion probe band at 790 cm−1 of optical glass. This leads to a linear dependence of the ratio of the intensity of non‐overlapping analyte bands at 1003 cm−1 of ‐C‐N‐ vibrations in urea to the one of the 790 cm−1 immersion probe band on the concentration of urea in the test solution. The definable method parameters such as precision (repeatability and reproducibility), linearity, limit of detection (LoD), limit of quantitation (LoQ), and accuracy were determined. The quantitative Raman spectroscopy method is linear, precise within the range of determined concentrations from 0.75 to 2.00 M and can be used to calculate the kinetics of allantoin formation. Using thiourea as an example, it is shown that despite the partial overlap of the analyte band at 730 cm−1 of the ‐C=S vibrations of thiourea with the immersion probe band at 790 cm−1, the method to determine thiourea in the reaction of 4,5‐dihydroxyimidazolidine‐2‐thione preparation is also linear and precise in the range of determined concentrations from 0.10 to 1.57 M.

Synthesis and Characterization of Hierarchically Porous Carbon Anodes from Furfural Biorefinery Residues for Sustainable Lithium-Ion Batteries

This study aims to valorize abundant lignocellulosic residues from furfural biorefineries into hierarchically porous carbon anodes for sustainable lithium-ion batteries (LIBs). Simultaneously, it addresses the growing demand for high-performance anode materials by leveraging renewable waste feedstocks. Sugarcane bagasse waste residues obtained after furfural extraction were used as the precursor. The furfural-derived bagasse residue (FDBR) underwent pyrolysis at 700 °C to produce a carbon-rich char, which was further activated using KOH and steam at 900 °C for 15-60minutes to enhance porosity development. Comprehensive physicochemical characterizations, including proximate analysis, N2 adsorption-desorption, SEM-EDX, FTIR, and TGA/DTG, and Raman spectroscopy were performed to evaluate the properties of the synthesized activated carbons. The results demonstrated the successful generation of high surface area (405.8 m2/g) activated carbons with a hierarchical pore structure comprising micropores and mesopores. SEM and EDX analyses revealed a uniform, porous morphology enriched with 10.41% at oxygen-containing functional groups. FTIR spectra confirmed the presence of hydroxyls, carbonyls, and carboxylic acid groups, beneficial for pseudocapacitive charge storage. The Raman analysis revealed a highly disordered and amorphous carbon structure with a significant concentration of defects, as evidenced by a high-intensity ratio (ID/IG ≈ 1.2-1.4) of the disordered carbon band to the graphitic band. The activated carbons exhibited a high initial discharge capacity of 1055mAh/g in lithium half-cells, significantly exceeding the theoretical limit of commercial graphite anodes (372mAh/g). This superior capacity was attributed to the high surface area, hierarchical porosity, and pseudocapacitive contributions from the oxygen functionalities. However, rapid capacity fading from 1055 to ~250mAh/g was observed over 100 cycles at a C/2 rate. The capacity retention stabilized at ~88% after 47 cycles, indicating irreversible capacity losses. These limitations were ascribed to the disordered amorphous structure, instability of the solid-electrolyte interphase, lithium trapping by oxygen groups, and structural changes during cycling. Optimizing activation conditions, incorporating conductive additives/coatings, exploring alternative binders, and surface functionalization are proposed to improve long-term cycling stability. Overall, this study demonstrates the feasibility of upcycling furfural biorefinery waste into sustainable LIB anodes while highlighting challenges and potential solutions for enhancing their electrochemical performance.

Functionalization of ZnO Nanoparticles and their Antimicrobial Activity: In Vitro

The precipitation process was used to synthesize ZnO nanoparticles (ZnO NPs), which were functionalized with fifteen amino acids and three surfactants. X-ray diffraction (XRD), field emission scanning microscopy (FESEM) with energy-dispersive X-ray spectroscopy, Fourier transformed infrared spectroscopy (FTIR), Raman spectroscopy, and UV-Vis spectroscopy were used to evaluate the synthesized and functionalized ZnO NPs. The characterization of the produced ZnO using XRD and FESEM revealed the development of a nanoscale hexagonal crystal, and the spectroscopic methods validated the presence of IR functional groups, Raman phase mode, and UV optical absorbance. The ZnO samples that had been functionalized demonstrated deformation in a surface morphology while maintaining chemical stability. The functionalization procedure effectively increases the inhibitory efficacy of NPs against Aspergillus Niger (Accession No. MZ435922) and Aspergillus Fumigatus (Accession No. MZ435863), as demonstrated by the antifungal activity. The findings of current work provide a foundation for improving the biological activity of NPs against fungi by modifying them with active medium and boosting their anti-microorganism and antioxidant activity.

Adsorption of trace metals onto different plastics during long-term exposure in an estuarine environment: Influence of time, stratified water column, and specific surface area

The pervasive increase of plastics in marine systems and subsequent trace metals (TM) adsorption represents a critical environmental challenge. This long-term study is first to investigate how duration of exposure and stratified water column impact TM adsorption on various plastics in an estuary. We exposed polypropylene (PP), polyethylene (PE), poly(ethylene terephthalate) (PET), and fluorinated ethylene propylene (FEP) to estuarine conditions, categorizing them into three distinct groups to capture diverse human activities: pre-production pellets (Pellets), single-use plastics (SUP) and laboratory plastics (Lab). Plastic and water samples were analyzed before deployment and 1, 4, 7 and 16 months after deployment at three depths in the stratified Krka River estuary (Croatia). We measured TM concentrations, pH and salinity in the water column, and adsorbed TM amounts on plastics. Additionally, we examined plastic sample surfaces by Raman spectroscopy and scanning electron microscopy. TM speciation was modeled from water column data to better explain adsorption processes. Statistical analysis indicates that Zn, Cd, Pb, Ni, and Co adsorption depends on both duration of exposure and stratified water column, while Cu is influenced solely by duration of exposure to estuarine environment. Adsorbed TM amounts varied significantly among the plastic groups (Pellets, SUP and Lab), but not among different polymer types (PP, PE, PET and FEP). A noteworthy observation was the difference in the results of statistical analysis when investigating TM amounts expressed by plastic sample mass and by plastic sample surface area. Results expressed by plastic sample mass showed a difference between SUP group versus Pellets and Lab groups, while results expressed by plastic sample surface area distinguished Pellets group compared to other two groups. Therefore, we suggest presenting TM adsorption results in similar studies both by plastic sample mass and by plastic sample surface area. This approach will improve the understanding of TM adsorption on plastics, and enable more effective comparisons among the scientific literature dealing with plastics of different specific surface areas.

E(n)-Equivariant cartesian tensor message passing interatomic potential.

Machine learning potential (MLP) has been a popular topic in recent years for its capability to replace expensive first-principles calculations in some large systems. Meanwhile, message passing networks have gained significant attention due to their remarkable accuracy, and a wave of message passing networks based on Cartesian coordinates has emerged. However, the information of the node in these models is usually limited to scalars, and vectors. In this work, we propose High-order Tensor message Passing interatomic Potential (HotPP), an E(n) equivariant message passing neural network that extends the node embedding and message to an arbitrary order tensor. By performing some basic equivariant operations, high order tensors can be coupled very simply and thus the model can make direct predictions of high-order tensors such as dipole moments and polarizabilities without any modifications. The tests in several datasets show that HotPP not only achieves high accuracy in predicting target properties, but also successfully performs tasks such as calculating phonon spectra, infrared spectra, and Raman spectra, demonstrating its potential as a tool for future research.

Effects of thermal and laser annealing on the structure of Ge2Sb2Te5 thin films

In this study, we used Raman spectroscopy to compare the local structure of Ge2Sb2Te5 (GST) thin films with thicknesses of 90 nm and 271 nm that were crystallized through thermal annealing and laser radiation (laser annealing) during the recording of Raman spectra in situ. We found that for all crystallized films, the position of the main peaks in the Raman spectra was almost the same, and their structure corresponded to a hexagonal close packed state. It is noteworthy that the full width at half maximum (FWHM) of the main peaks varies considerably depending on the crystallization method used.

Hydrothermal synthesis of La0.5Sr0.5MnO3 nanostructures for enhanced CO oxidation

This study focuses on the synthesis and characterization of La0.5Sr0.5MnO3 (LSMO) perovskite nanostructures via the hydrothermal method and their catalytic performance evaluation in CO oxidation. Structural analysis using techniques like XRD, FE-SEM, FTIR, and Raman spectroscopy analysis verified the development of LSMO nanostructures exhibiting a rhombohedral phase configuration. The catalytic activity of the annealed LSMO nanostructures was assessed, demonstrating significant CO conversion efficiency attributed to structural modifications enhancing catalytic performance. These findings highlight the potential of LSMO perovskite nanostructures as efficient catalysts for CO oxidation.

A Unified Prediction Strategy for Angle‐Resolved Polarized Raman Response of Black Phosphorus

AbstractPredicting the angle‐resolved polarized Raman spectroscopy (ARPRS) response of anisotropic layered materials (ALMs) is the ultimate goal in the field of ARPRS research. So far, multiple physical mechanisms are studied on the representative black phosphorus (BP) to understand the intricate ARPRS response. However, the lack of a complete physical picture of the response modulation has hindered progress in response prediction. Herein, using BP as an example, a unified strategy for predicting the thickness‐dependent ARPRS response of ALMs is proposed. Crucially, with only one ARPRS measurement of a bulk ALM of interest, the response of nanoflakes of any thickness can be predicted. This is achieved based on the core concept of intrinsic Raman anisotropy (RA). Integrated experiments, analysis, and calculations reveal that the response of bulk BP is reshaped by the rarely noticed anisotropic absorption effect, which leads to an unique thickness‐independent constant modulation. Therefore, the interference‐free bulk counterpart of ALMs can serve as an ideal platform for accurately accessing intrinsic RA. This work provides a new paradigm for ARPRS research and paves the way for profound study of intrinsic RA.

The effect of A-site cations on charge-carrier mobility in Fe-rich amphiboles

Abstract Elucidating the high-temperature behavior of rock-forming minerals such as amphiboles (AB2C5 T8O22W2) is critical for the understanding of large-scale geological processes in the lithosphere and, in particular, the development of high conductivity in the Earth’s interior. Recently, we have shown that at elevated temperatures, CFe-bearing amphiboles with a vacant A site develop two types of charge carriers: (1) small polarons and (2) delocalized H+ ions. To elucidate the effect of A-site cations on the formation and stability of charge carriers within the amphibole structure, here we analyzed synthetic potassic-ferro-richterite as a model Fe-rich amphibole with a fully occupied A site via in situ temperature-dependent Raman spectroscopy. We further compare the results from in situ time-dependent Raman-scattering experiments on pre-heated and rapidly quenched potassic-ferro-richterite and riebeckite as a model Fe-rich amphibole with a vacant A site. We show that the presence of A-site cations (1) reduces the activation temperature of mobile polarons and delocalized H+ cations; (2) decreases the magnitude of the polaron dipole moment; (3) slows down the process of re-localization of electrons on cooling; and (4) makes the electrons inert to rapid change in external conditions, supporting the persistence of a metastable state of pre-activated delocalized electrons even at room temperature. Our results have important geological implications demonstrating that the A-site cations may control the depth of development of high conductivity in subducted amphibole-bearing rocks. Moreover, from the viewpoint of mineral-inspired materials science, our results suggest that the amphibole-structure type has great potential for designing functional materials with tunable anisotropic-conductivity properties.

Inhalable explosive nanosensor for real-time visual monitoring of therapeutic effects of lung cancer

Lung cancer, as one of the major diseases that endanger human health, has a very high fatality rate. Consequently, effective evaluation of clinical treatment outcomes for lung cancer is crucial for the formulation of subsequent treatment plans for patients. In this work, we utilized amorphous calcium carbonate nanoparticles (CaCO3 NPs) as sources of calcium ions (Ca2+) to develop CPs (CaCO3@PDA) core–shell nanoprobes. Concurrently, we functionalized the surface of gold nanoparticles with Cy5.5-peptide, AS1411, and (4-aminosulfonylphenyl) boronic acid (4-APBA) to produce APAAs (Au NPs@pep-AS1411-(4-APBA)), which were further assembled with CPs using PEG to construct an innovative explosive nanosensor, CPAs (CaCO3@PDA-APAAs). The CPs component of the nanosensor could cause the release of a substantial amount of Ca2+ in response to the tumor microenvironment (TME), which in turn induced cellular Ca2+ overload and subsequent apoptosis. This event triggers caspase-3 activation, causing the cleavage of a specific peptide sequence (DEVD), resulting in the fluorescence signal being reinstated. Additionally, the 4-APBA moiety on the probe interacted with H2O2 resulting in alterations in surface-enhanced Raman spectroscopy (SERS) signals, which aided in the detection of reactive oxygen species (ROS) during the physiological processes. By utilizing atomization, the nanoprobes were strategically deposited in the affected lung regions to enhance the fluorescence imaging capabilities and effectively mirror the therapeutic outcomes. Overall, the CPAs explosive nanosensor has a potential in advancing the non-invasive visual monitoring of lung cancer prognosis and can be a valuable tool in ongoing efforts to improve the management of this challenging disease.

Unveiling the enhanced hydrogen evolution performance of ternary heterostructures Mo5O14-Y(OH)3-CoMoO4/CF electrocatalysis

The challenge in electrocatalysis lies in finding stable and efficient catalysts for hydrogen evolution, especially those based on non-noble metals. Herein, the Mo5O14-Y(OH)3-CoMoO4/CF (CF stands for cobalt foam) catalyst rich in ternary heterostructures have been successfully synthesized. The catalyst is composed of cumin-like nanoparticles randomly dispersed on microcolumns. This unique structure ensures both its electrocatalytic activity and structural stability. Electrochemical tests demonstrate exceptional water splitting capabilities, with overpotentials of just 40 mV at 10 mA cm−2 (j10) and 219 mV at 1000 mA cm−2 (j1000). Furthermore, the catalyst shows minimal performance degradation after long-term testing, maintaining stable electrochemical performance for 60 h at j10 and 18 h at j800. Surface energy calculations and scanning electron microscopy (SEM) indicate that yttrium(Y) promotes the formation of cumin-like nanoparticles. Density functional theory (DFT) analysis, along with in situ Raman spectroscopy, suggests that the interaction among the three metals forms Mo5O14-Y(OH)3-CoMoO4 ternary heterostructures, effectively reducing the energy barrier for the hydrogen evolution reaction (HER). Notably, the Y sites in the CoMoO4-Y(OH)3 heterostructure exhibit the lowest hydrogen adsorption free energy (ΔGH⁎: −0.31 eV), making them the primary active sites for Mo5O14-Y(OH)3-CoMoO4/CF.

Characterization of corrosion products formed in high-strength dual-phase steels under an accelerated corrosion test

There are some researches in the literature on the mechanical characteristics of dual-phase (DP) steels used in the automotive industry, but there is no comprehensive research on the corrosion behavior of these steels. In this work, the corrosion behavior of DP steels (DP440, DP590, DP980) exposed to two cycles of accelerated corrosion testing in accordance with Ford CETP 00.00-L-467 was observed. Raman and X-ray diffraction (XRD) techniques were used to classify the corrosion products, and the morphology of the samples was studied using a scanning electron microscope (SEM). Goethite and haematite were the primary chemical compounds determined. In high-mechanical strength DP steels, akaganeite was also identified in corroded specimens. The compounds formed due to corrosion were revealed by SEM images. In this work, according to the results of Raman spectroscopy, which was employed for the first time to reveal corrosion products in high-strength dual-phase steels, it was discovered that corrosion products increased with increasing mechanical strength due to an increasing martensite phase volume percentage. Polarization tests were carried out to support the electrochemical data reported by the Raman analysis. Similarly, an increase in the amount of martensite phase in the microstructure led to a decrease in the material’s corrosion resistance. Polarization experiments were carried out to support the electrochemical data interpreted by Raman analysis. In addition, an increase in the amount of martensite phase in the microstructure led to a decrease in the corrosion resistance of the material. In addition, information regarding the material’s electrochemical performance was obtained through Raman analysis. As shown by Raman, XRD, and polarization tests, the increase in corrosion products formed due to the increase in the amount of martensite led to a decrease in corrosion resistance.

Dual-mode electrochemical and SERS detection of PFAS using functional porous substrate

Human activity is the cause of the continuous and gradual grooving of environmental contaminants, where some released toxic and dangerous compounds cannot be degraded under natural conditions, resulting in a serious safety issue. Among them are the widely occurring water-soluble perfluoroalkyl and polyfluoroalkyl substances (PFAS), sometimes called “forever chemicals” because of the impossibility of their natural degradation. Hence, a reliable, expressive, and simple method should be developed to monitor and eliminate the risks associated with these compounds. In this study, we propose a simple, express, and portable detection method for water-soluble fluoro-alkyl compounds (PFOA and GenX) using mutually complementary methods: electrochemical impedance spectroscopy (EIS) and surface-enhanced Raman spectroscopy (SERS). To implement our method, we developed special substrates based on porous silicon with a top-deposited plasmon-active Au layer by subsequently grafting –C6H4NH2 chemical moieties to provide surface affinity toward negatively charged water-soluble PFAS. Subsequent EIS utilization allows us to perform semiquantitative detection of PFOA and GenX up to 10−10 M concentration because surface entrapping of PFAS leads to a significant increase in the electrode–electrolyte charge-transfer resistance. However, distinguishing by EIS whether even PFAS were entrapped was impossible, and thus the substrates were subsequently subjected to SERS measurements (allowed by surface plasmon activity due to the presence of a porous Au layer), clearly indicating the appearance of characteristic C–F vibration bands.

Multi-stage magmatic–hydrothermal evolution of nepheline pegmatite: Insights from the mineralogy and geochronology of a zircon megacryst from the Yilanlike nepheline pegmatite, South Tianshan

Magmatic–hydrothermal evolution plays a key role in the formation of peralkaline rocks and associated zirconium and rare earth element (REE) mineralization. Zircon is a common mineral in peralkaline rocks and can record invaluable information about the magmatic–hydrothermal evolution of these systems. To help better constrain the magmatic–hydrothermal evolution of and Zr enrichment processes in peralkaline systems, we characterized the mineralogy and geochronology of a texturally complex zircon megacryst from the rare metal mineralized Yilanlike nepheline pegmatite in the South Tianshan. Here we present laser Raman spectra, in situ elemental data, and U–Pb geochronological data for the zircon megacryst to constrain the age and magmatic–hydrothermal evolution of this nepheline pegmatite. Three types of zircon domains (Zrn-I, Zrn-II, and Zrn-III) are distinguished based on their morphological and geochemical characteristics. Zrn-I has well-developed oscillatory zoning, REE patterns similar to magmatic zircon, high Th/U ratios (0.09–0.47), and concordant U–Pb ages, indicative of a magmatic origin. Zrn-II is characterized by weak oscillatory and patchy zoning, low full width at half maximum (FWHM) values (6.58–14.86 cm−1), and low trace-element contents (e.g., Nb = 0.16–0.92 ppm, Ta = 0.13–0.54 ppm, U = 195.77–812.92 ppm, Th = 15.85–158.95 ppm, and total REE = 13.00–187.75 ppm), indicative of a recrystallized origin as this process generates heterogeneous zoning, heals the zircon crystal lattice, and lowers trace-element contents. Concordant U–Pb ages and low Th/U ratios (0.05–0.26), combined with moderate Ce/Ce* and (Sm/La)N ratios (0.38–33.96 and 1.34–27.73, respectively), which are characteristic of the magmatic–hydrothermal transition, indicate that Zrn-II recrystallized in the presence of hydrothermal fluids. Zrn-III is characterized by “spongy” textures, thorite inclusions, high FWHM values (6.58–47.87), relatively high contents of total REE (14.79–962.05 ppm), and discordant U–Pb ages, suggestive of an origin related to the hydrothermal alteration of earlier zircons. Results of U–Pb dating of Zrn-I and -II yield weighted concordant ages of 286.9 ± 1.9 Ma (MSWD = 1.5, n = 23) and 279.3 ± 2.3 Ma (MSWD = 0.24, n = 20), respectively, whereas the U–Pb results for Zrn-III are largely discordant. Based on these textural, geochemical, and geochronological results, a multi-stage process for the formation of the zircon megacryst and nepheline pegmatite is proposed. First, the parent magma of the nepheline pegmatite was emplaced and the zircon megacryst crystallized at ca. 286.9 Ma (represented by Zrn-I). As the magma differentiated, hydrothermal fluids derived from the evolved magma recrystallized Zrn-I to Zrn-II at ca. 279.3 Ma. Finally, a second hydrothermal event altered Zrn-I and -II to form Zrn-III. Given the low concentrations of UO2, ThO2, and Y2O3 in Zrn-II, and the CHARAC behavior of Zr and Hf, the fluid that formed this zircon variety likely had relatively low F contents. This multi-stage magmatic–hydrothermal evolution likely played an essential role in concentrating Zr and generating the Zr mineralization. Zirconium is primarily enriched via magmatic crystallization, as illustrated by the high abundances of Zrn-I in the Yilanlike nepheline pegmatite. The presence of recrystallized zircon (Zrn-II and Zrn-III) suggests that hydrothermal recrystallization may have also facilitated the enrichment of Zr. It is, therefore, suggested that both magmatic and hydrothermal processes contributed to the enrichment of Zr in the Yilanlike nepheline pegmatite.