Raman Spectroscopy Research Articles

Molecular investigation of bamboo during stress relaxation using custom-built mechanical loading platform coupled with Raman spectroscopy

Bamboo holds significant potential as a substitute for plastics. Stress relaxation is a critical property during the fixation stage of plastic formation for bamboo products intended to replace plastic. However, research on this topic has been limited. In this study, a custom-built mechanical loading platform coupled with Raman spectroscopy was acquired during stress relaxation of bamboo under different humidity levels. Results reveal variations in stress relaxation patterns based on node position, radial location, and humidity, along with changes in cellulose molecules in response to these factors. Specifically, stress relaxation modulus in bamboo decreases from the outer to the inner part, increases in the presence of node structures, and decreases with increasing humidity. The shifts in Raman spectral bands exhibit significant changes in response to variations in stress and humidity. The elongation of cellulose chain bands at 1097 cm−1 in the Raman spectrum shows an increasing trend during stress relaxation, with larger band shifts observed at lower humidity. Simulations of cellulose molecular stretching show a stronger stress response at lower moisture content, with a maximum stress of 0.85 GPa for cellulose at 3.3 % moisture content, compared to 0.79 GPa at 7.8 % moisture content. These findings suggest a novel approach for the molecular investigation of materials during stress relaxation, which is crucial for the plasticity processing of bamboo.

The role of iron(II) excess and phosphate to synthesize hydroxychloride green rust

Green rust (GR) is a chemically reactive mineral of interest for environmental remediation. However, the lack of stability of this compound is a major drawback for practical applications. In this study, the precipitation of hydroxychloride green rust type 1 (GR1Cl) from soluble FeII and FeIII species was studied by analyzing pH titration curves and employing XRD, Raman and Mössbauer spectroscopies to find optimal conditions for synthesizing GR1Cl. Using the stoichiometric condition for FeII-FeIII corresponding to the [FeII3FeIII(OH)8]Cl compound, FeIIIO(OH)2.9Cl0.1 was formed in a first step during the addition of NaOH and then transformed into a mixture of GR1Cl and Fe3O4. The addition of phosphate anions (PO4) at a molar ratio PO4: Fe = 1: 10 in the initial solution was shown to avoid the formation of undesired magnetite. Interestingly, GR1Cl was also the only product without adding PO4 using an excess of FeII species in solution, i.e. for an initial ferric molar fraction x = FeIII: Fetot of 0.2. First experimental evidences of a hydroxyphosphate green rust type 2 GR2PO4 were also provided by XRD and Raman spectroscopy. Therefore, this work may attract interest for a better understanding of the geochemical cycle of iron and phosphate in natural environments such as hydromorphic soils or hydrothermal chimneys where fougerite, the mineral homologue of synthetic GR, is supposed to play a significant role.

Corrosion resistance and wear behavior of CoCrFeNiMn@Gr high entropy alloy-based composite coatings prepared by laser cladding

In this study, we utilize laser cladding to apply a CoCrFeNiMn HEA with 2 wt.% few-layer graphene (Gr) coating onto the surface of Q235B mild steel. Alcohol stirring method was used for HEA and Gr preparation of composite powder. Raman spectroscopy and energy dispersion spectroscope (EDS) indicate the successful mixing of HEA and Gr powders, with Gr adhering to the surface of the HEA powder in a lamellar structure. The X-ray diffraction (XRD), scanning electron microscope (SEM), EDS, and Electron backscatter diffraction (EBSD) analyses revealed that grain refinement and the formation of fine carbide-hard phases in the HEA/Gr coating improve microhardness and wear resistance. The average Schmidt factors of the coating decreased from 0.47 to 0.45 with the addition of Gr, indicating enhanced resistance to plastic deformation and anisotropy. Nanoindentation experiments demonstrated that the HEA/Gr coatings exhibit superior resistance to plastic deformation, effectively enhancing the coating’s durability against spalling under stress and wear conditions. The microhardness of the HEA/Gr coating increased by 99.25%, and the wear rate decreased by 86.31% compared to the HEA coating alone. The open circuit potential (OCP), linear polarization curve, Tafel curves, electrochemical impedance spectroscopy (EIS), and Mott-Schottky tests all indicated that the HEA/Gr coating possesses superior corrosion resistance. X-ray Photoelectron Spectroscopy (XPS) results suggest that the passivation film of the HEA/Gr coating, which contains more oxides and less hydroxide, is more protective and denser, thereby slowing the corrosion rate.

Graphite and multi-layer graphene from a low molecular weight carbon source

While carbonaceous structures formed by pyrolysis of macromolecular carbon sources with silicates are well described in the literature, information on the structure of carbons obtained in the similar way from low molecular weight (LMW) carbon sources is not sufficient. This study is therefore aimed at characterizing the material obtained by pyrolyzing (1300 °C; Ar atmosphere) montmorillonite containing ∼25-50 wt.% LMW cations as a carbon source. Pyrolyzed samples contained ∼5-20 wt.% carbon, and thermogravimetric and elemental analysis showed a higher yield for a higher original amount of the LMW carbon source. In addition to amorphous carbon, graphite was formed during pyrolysis, as confirmed by X-ray diffraction analysis, Raman spectroscopy, and X-ray photoelectron spectroscopy. The presence of graphene-based nanomaterial, specifically multi-layer graphene, was revealed by transmission electron microscopy (TEM). Electrical conductivity of the silicate/carbon material reached ∼35 S·m-1. Raman spectra and TEM images are similar to those from studies describing the use of macromolecular carbon sources. LMW compounds are a sufficient source of carbon for the preparation of electrically conductive materials containing graphite and multi-layer graphene.

Hydrogen resistance of reduced graphene oxide coatings prepared by electrophoretic deposition on duplex stainless steel

In this study, reduced graphene oxide (rGO) coatings were fabricated on duplex stainless steel (DSS) substrates using the electrophoretic deposition (EPD) method to evaluate their hydrogen resistance performance. The successful fabrication of rGO coatings was confirmed using Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Spectroscopy (XPS). The structural characteristics were characterized using Raman spectroscopy and X-ray Diffraction (XRD). The results indicate that the EPD voltage is a crucial factor affecting the surface quality of and hydrogen resistance performance of rGO. Lower voltages resulted in lower degrees of rGO reduction and higher surface wrinkle density, while higher voltages caused bubble formation, significantly degrading the coating quality and hydrogen resistance performance. The optimal hydrogen resistance was achieved at an EPD voltage of 7.5V and a deposition time of 6 minutes. Electrochemical hydrogen charging tests and thermal desorption analysis (TDA) demonstrated that rGO coatings prepared under optimal conditions exhibited excellent hydrogen resistance efficiency, significantly reducing hydrogen atom penetration in hydrogen environments. The study further revealed that bubble formation significantly reduces the hydrogen resistance of rGO, which is attributed to increased interlayer spacing and the loss of the “labyrinth effect”.

Ultramarine blue containing paint layers: Further study of the photo-catalytic degradation of binding media

Photo-catalytic degradation of a linseed oil binder by natural ultramarine (Lapis Lazuli or Lazurite) and Sodalite in paint layers was studied. Both pigments degrade the binder under xenon arc exposure, leading to erosion of the binder at the surface, increased roughness, light scattering and desaturation of the color. Both pigments behave similarly to synthetic ultramarine blue studied earlier. The results for Sodalite provide further proof that the zeolitic nature of the aluminosilicate cage causes the catalytic degradation and that the enclathrated polysulfur radical anions S2-. and S3-. trapped inside the cage are not responsible for the catalytic action. Relatively stable synthetic binders are less affected by the presence of synthetic ultramarine blue. The paints were aged in a xenon arc apparatus using a simulated indoor environment (radiation > ca. 320 nm). The samples were analyzed using diffuse reflectance spectroscopy in the UV–vis and short wavelength infrared (SWIR) ranges, Raman spectroscopy, field-emission gun scanning electron microscopy (FEG-SEM) and FTIR.

Characterization of thin oxide layers formed by Ti-Nb Alloy anodization

Ti-Nb alloys are gaining more prominence in the industrial and scientific environment due to their high biocompatibility, mechanical strength/weight ratio, and exceptional corrosion resistance compared to other metallic materials. Metals exhibiting this passivation characteristic are known as metal valves and may exhibit semiconductive or insulating oxides. Controlling the growth of distinct thickness layer films is possible through tunning anodization conditions. In this work, a Ti-Nb binary system is anodized, and the grown oxide layer is comprehensively characterized using ellipsometry based on its optical properties and thickness at different applied potentials. Confocal Microscopy assessed their surface roughness, and SEM/EDS probed the surface material's elemental composition. CF-LIBS successfully confirmed the 70/30 composition of the Ti-Nb alloy. Raman spectra have detected the presence of amorphous TiO2 and Nb2O5 at potentials higher than 80V, 100V, and 120V. Finally, a linear dependence of the oxide thickness with the applied potential was observed.

Silver doping effect on the electrochromic performance of the WO3 thin films produced by thermal evaporation in vacuum

Ag doped WO3 thin films are successfully fabricated by thermal evaporation method in vacuum as precursor, and then annealed at 450 °C in nitrogen gases atmosphere. Cyclic voltammetry, repeating chronoamperometry, chronocolumetry and optical transmittance are recorded in 1 M LiClO4/propylene carbonate electrolyte. The color of the WO3 thin films changes from transparent to the blue under the applied potential of -1.8 and +1.9 V. XRD studies show that all the films have a polycrystalline structure of WO3. The molecular formation is also confirmed by Raman and X-Ray photoelectron spectroscopy (XPS). The EDS elemental mappings clearly confirm the homogeneous distribution of Ag, W and O elements into the WO3 network. From the optical studies, indirect band gap energy of the WO3 decreases as Ag doping level increases. The best coloration and bleaching times (2.33 and 1.25 s) are obtained for the Ag(2%):WO3 thin films, compared to the pure WO3 (3.79 and 1.96 s). The produced WO3 films exhibit high reversibility (39.6/69.1%), high coloration efficiency values (26.3/141.2 cm2/C), and good cycling stability. From the EIS measurements, the charge-transfer resistance is Ag(2%):WO3 < the pure WO3 < Ag(5%):WO3 < Ag(8%):WO3, which means that Ag(2%):WO3 has the biggest electrochemically active surface area. Electronic energy levels of the pure WO3 and the Ag:WO3 thin films are also given. From the Mott-Schottky studies, it is determined that the donor concentration of the materials is of the order of 1014-1015 cm−3. In the literature, there are very limited studies related to electrochromic thin films by thermal evaporation in vacuum. In this sense, the reported results in this study are promising for the electrochromic applications.

Efficient activation of peroxyacetic acid by cobalt-iron alloy/oxide heterojunctions anchored in defect-rich biochar for pesticide degradation in water: Unravelling the radical-unradical mechanism

The activation processes of peracetic acid (PAA-AOPs) have garnered significant attention in wastewater treatment. In this study, an amorphous carbon-modified bimetallic CoFe alloy/oxide catalyst (CoFe@DBCx-y, where x represents biomass mass and y represents pyrolysis temperature) was developed to activate PAA for the degradation of organochlorine pesticides (OCPs). Due to the size effect, biochar dynamically regulates the particle size of metal species, which is influenced by the pyrolysis temperature. Among these systems, the CoFeDBC2.0–700/PAA oxidation system effectively removed 95.7 % of 2,4-dichlorophenoxyacetic acid (2,4-D), exhibiting a kinetic constant 1.7 times higher than that of the Nano/PAA system. Furthermore, quenching experiments and electron paramagnetic resonance (EPR) analysis revealed that high-valent metal oxides (MIV = O) and singlet oxygen (1O2) are the primary active species responsible for the removal of 2,4-D, whereas organic radicals (RO·) and hydroxyl radicals (·OH) play a secondary role. Electrochemical and Raman spectroscopy tests revealed the formation of a metastable surface complex (≡Co(III)–OO(O)CCH3) between PAA and the catalyst, which acted as an intermediate oxidant to generate reactive oxygen species (ROS) through a chain reaction. Carbon defects in the biochar functioned as an electron source, continuously replenishing the electrons consumed in the reaction and facilitating the valence cycling between Co and Fe. This study provides new insights into the remediation of pesticide-contaminated wastewater using PAA-AOPs with heterogeneous bimetallic carbon-based catalysts.

Continuous lattice oxygen participation of NiFe stack anode for Sustainable water Splitting

Non-noble anode catalysts exhibit insufficient activity and stability for anion exchange membrane water electrolysis (AEMWE). Accordingly, we propose an electrolyte additive strategy involving NiFe-layered double hydroxide. In situ Raman spectroscopy and 18O isotope labeling experiments reveal that Fe ions in the electrolyte change the oxygen evolution reaction mechanism from adsorbate evolution to the lattice oxygen participation mechanism (LOM). These Fe ions continuously refill Fe vacancies owing to facile metal dissolution via the LOM. In a unit cell, we achieve an excellent cell voltage of 1.73 V and energy conversion efficiency (ECE) of 69.4 % at 3.0 A cm−2, meeting the target set by the U.S. Department of Energy (1.80 V and 69.0 % ECE). Our optimized membrane electrode assembly enhances the cell activity (1.567 V at 1.0 A cm−2; ECE = 76.5 %) and stability (0.125 mVcell h−1 at 0.5 A cm−2 for 500 h) with a 100 cm2 AEMWE stack.

Electronic, thermodynamic, NLO, and spectroscopic properties of OAFLC compounds via DFT: A focus on 1F6B, 1F6Bi, 1F6BiN, and 1F6BN

This study presents a comprehensive quantum mechanical investigation of four novel liquid crystalline compounds: 1F6B, 1F6Bi, 1F6BiN, and 1F6BN. Using Density Functional Theory (DFT) with the B3LYP functional and 6-311G(d,p) basis set, we optimized the molecular geometries and analyzed their electronic and vibrational properties. Atomic Polar Tensor (APT) charge analysis showed significant charge distributions. Electrostatic potential (ESP) mapping identified potential reactive sites, while Electron Localization Function (ELF) and Localized Orbital Locator (LOL) analyses depicted the electron density distributions. Thermodynamic parameters indicated the compounds’ vibrational stability and responsiveness to thermal changes. Non-linear optical (NLO) properties were characterized by significant dipole moments and polarizabilities, suggesting potential in optoelectronic applications. Frontier molecular orbital analysis indicated stability with HOMO-LUMO gaps ranging from 4.15 to 4.64 eV. UV–Vis spectra revealed key electronic transitions, while Raman spectroscopy detailed various vibrational modes. The study offers valuable insights into the molecular behavior of these compounds, laying the groundwork for their future applications in material science and advanced technologies.

Surface-enhanced Raman spectroscopy substrates for monitoring antibiotics in dairy products: Mechanisms, advances, and prospects.

Antibiotic residues in dairy products have become an undeniable threat to human health. Surface-enhanced Raman spectroscopy (SERS) has been widely used in efficiently detecting antibiotics because of its characteristics including fast response, high resolution, and strong resistance to moisture interference. However, as a core part of SERS technology, the design principle and detection performance of enhanced substrates used in monitoring antibiotics in dairy products have not yet received enough attention. Thus, it is necessary to give a critical review of the recent developments of SERS substrates for monitoring antibiotics in dairy products, which can be expected to provide inspiration for the efficient utilization of SERS technology. In this work, advances in various SERS substrates applied in sensing antibiotics in dairy products were comprehensively reviewed. First, the enhancement mechanisms were introduced in detail. Significantly, the types of enhanced materials (plasmonic metal particles [PMPs], PMPs/semiconductor composite materials) and biometric design strategies including immunoassay, aptamer, and molecularly imprinted polymers-based SERS biosensors applied in dairy products were systematically summarized for the first time. Meanwhile, the performance of SERS substrates used for the detection of antibiotics in dairy products was addressed from the aspects of dynamic linear range and detection restriction strategy. Finally, the conclusions, challenges, and future prospects of SERS substrates for antibiotic monitoring in dairy products were deeply discussed, which also provide new opinions and key points for constructing SERS substrates applied in complex food matrix in the future.

Identification of graphite with perfect rhombohedral stacking by electronic Raman scattering

Rhombohedral graphite (RG) shows strong correlations in its topological flat band and is pivotal for exploring emergent, correlated electronic phenomena. One key advantage is the enhancement of electronic interactions with the increase in the number of rhombohedrally stacked graphene layers. Increasing thickness also leads to an exponential increase in the number of stacking configurations, necessitating a precise method to identify flawless rhombohedral stackings. Overcoming this challenge is difficult because the established technique for stacking sequence identification, based on phonon originated Raman processes (e.g. the 2D peak), fails in thick RG samples. We demonstrate that the strong layer dependence of the band structure can be harnessed to identify RG without stacking faults. For thicknesses ranging from 3 to 12 layers, we show that each perfect RG structure presents distinctive peak positions in electronic Raman scattering (ERS), directly fingerprinting the flawless stacking. This measurement can be carried out using a conventional confocal Raman spectrometer at room temperature, using visible excitation wavelengths. Consequently, this overcomes the identification challenge by providing a simple and fast optical measurement technique, thereby helping to establish RG as a platform for studying strong correlations in one of the simplest crystals possible.

Application of Raman spectroscopy and machine learning for Candida auris identification and characterization.

Currently, combating Candida auris infections and transmission is challenging due to the lack of efficient identification and characterization methods for this species. To address these challenges, our study presents a novel approach that utilizes Raman spectroscopy and artificial intelligence to achieve precise identification and characterization of C. auris at the singe-cell level. It can accurately identify a single cell from the four C. auris clades. Additionally, we developed machine learning models designed to detect antifungal resistance in C. auris cells and differentiate between two distinct phenotypes based on the single-cell Raman spectrum. We also constructed prediction models for detecting aggregating and filamentous cells in C. auris, both of which are closely linked to its virulence. These results underscore the merits of Raman spectroscopy in the identification and characterization of C. auris, promising improved outcomes in the battle against C. auris infections and transmission.

Surface-Enhanced Raman Scattering Combined with Machine Learning for Rapid and Sensitive Detection of Anti-SARS-CoV-2 IgG

This work reports an efficient method to detect SARS-CoV-2 antibodies in blood samples based on SERS combined with a machine learning tool. For this purpose, gold nanoparticles directly conjugated with spike protein were used in human blood samples to identify anti-SARS-CoV-2 antibodies. The comprehensive database utilized Raman spectra from all 594 blood serum samples. Machine learning investigations were carried out using the Scikit-Learn library and were implemented in Python, and the characteristics of Raman spectra of positive and negative SARS-CoV-2 samples were extracted using the Uniform Manifold Approximation and Projection (UMAP) technique. The machine learning models used were k-Nearest Neighbors (kNN), Support Vector Machine (SVM), Decision Trees (DTs), logistic regression (LR), and Light Gradient Boosting Machine (LightGBM). The kNN model led to a sensitivity of 0.943, specificity of 0.9275, and accuracy of 0.9377. This study showed that combining Raman spectroscopy and a machine algorithm can be an effective diagnostic method. Furthermore, we highlighted the advantages and disadvantages of each algorithm, providing valuable information for future research.

Electrochemical Formation of C2+ Products Steered by Bridge-Bonded *CO Confined by *OH Domains.

During the electrochemical CO2 reduction reaction (eCO2RR) on copper catalysts, linear-bonded CO (*COL) is commonly regarded as the key intermediate for the CO-CO coupling step, which leads to the formation of multicarbon products. In this work, we unveil the significant role of bridge-bonded *CO (*COB) as an active species. By combining in situ Raman spectroscopy, gas and liquid chromatography, and density functional theory (DFT) simulations, we show that adsorbed *OH domains displace *COL to *COB. The electroreduction of a 12CO+13CO2 cofeed demonstrates that *COB distinctly favors the production of acetate and 1-propanol, while *COL favors ethylene and ethanol formation. This work enhances our understanding of the mechanistic intricacies of eCO(2)RR and suggests new directions for designing operational conditions by modifying the competitive adsorption of surface species, thereby steering the reaction toward specific multicarbon products.

Constructing Ag/Cu2O interface for efficient neutral CO2 electroreduction to C2H4.

Neutral CO2 electroreduction to multi-carbons (C2+) offers a promising pathway to reduce the CO2 and energy losses originating from the carbonate formation. However, the sluggish kinetics of C-C coupling brings a significant challenge of achieving high selectivity of a single product (such as ethylene), especially at industrial-relevant current densities (> 300 mA cm-2). Here, we reported an optimized Ag-Cu2O interfacial catalyst that exhibited C2+ Faradaic efficiency (FE) of 73.6% at 650 mA cm-2 in a flow cell. Remarkably, it obtained FEC2H4 of 66.0% with a partial current density of 429.1 mA cm-2, making it stand out among the reported Cu-based electrocatalysts. In situ Raman spectra uncovered that the Ag/Cu2O interfaces enabled a high coverage of *CO around the partially reduced Cu+/Cu0 active sites. Furthermore, theoretical calculations demonstrated the enhanced CO formation and C-C coupling at the Ag/Cu2O interface. This work reported an unprecedented neutral CO2 electroreduction to C2H4 performance and provided an in-depth comprehension of the role of the bimetallic interface.

Memristive Artificial Synapses Based on Brownmillerite for Endurable Weight Modulation.

Exploring a computing paradigm that blends memory and computation functions is essential for artificial synapses. While memristors for artificial synapses are widely studied due to their energy-efficient structures, random filament conduction in general memristors makes them less preferred for endurability in long-term synaptic modulation. Herein, the topotactic phase transition (TPT) in brownmillerite-phased (110)-SrCoO2.5 (SCO2.5) is harnessed to enhance the reversibility of oxygen ion migration through 1-D oxygen vacancy channels. By employing a heteroepitaxial structured 2-terminal configuration of Au/SCO2.5/SrRuO3/SrTiO3, the brownmillerite SCO2.5-based synapse artificial synapses are exploited. Demonstration of the TPT behavior is corroborated by comparing oxygen migration energy by density-functional theory calculations and experimental results, and by monitoring the voltage pulse-induced peak shift in the Raman spectra of SCO2.5. With the voltage pulse-driven TPT behaviors, it is reliably characterized by linear, symmetric, and endurable long-term potentiation and depression performances. Notably, the durability of the TPT-based weight control mechanism is demonstrated by achieving consistent and noise-free weight updates over 32 000 iterations across 640 cycles. Furthermore, learning performances based on deep neural networks and convolutional neural networks on various image datasets yielded very high recognition accuracy. The work offers valuable insights into designing memristive synapses that enable reliable weight updates in neural networks.

Producing Activated Biochar from the Reuse of Discarded Coffee Grounds with Enhanced Adsorptive Features Explored Towards the Stripping Voltammetric Sensing of Copper (II)

AbstractThis work aims to allocate coffee grounds waste to the production of biochar from pyrolysis under different temperatures (350 °C and 500 °C), to add value to it. The resulting materials were characterized by immediate, elemental, thermogravimetric analysis, SEM, FT‐IR, XRD and Raman spectroscopy. Additionally, the need to activate the biochar produced for the desired use was evaluated. The obtained biochars were applied in electroanalysis in the manufacture of modified carbon paste electrodes. This choice was made due to the possibility of reaching a high sensitivity towards the determination of Cu2+ ions. The differential pulse adsorptive anodic stripping voltammetry technique was applied to perform the Cu2+ determination and, in this case, several parameters were optimized, including biochar’ percentage, pH of pre‐accumulation step and reduction/stripping step, pre‐accumulation time, potential and time of reduction of adsorbed‐Cu2+. From this, the proposed modified electrode showed a linear voltammetric response towards Cu2+ in the range of 66.1 to 3997.3 ppb, with a limit of detection of 31.8 ppb, in addition to having been satisfactorily applied in the analysis of water samples (recoveries close to 100 %). Thus, demonstrating the potential for reuse of discarded coffee grounds for the preparation of activated biochar with outstanding electrochemical performance.

The Synergic Effect of h-MoO3, α-MoO3, and β-MoO3 Phase Mixture as a Solid Catalyst to Obtain Methyl Oleate.

Extensive research in the last few decades has conclusively demonstrated the significant influence of experimental conditions, surfactants, and synthesis methods on semiconductors' properties in technological applications. Therefore, in this study, the synthesis of molybdenum oxide (MoO3) was reported by the addition of 2.5 (MoO3_2.5), 5 (MoO3_5), 7.5 (MoO3_7.5), and 10 mL (MoO3_10) of nitric acid, obtaining the respective concentrations of 0.6, 1.10, 1.6, and 0.6 mol L-1. In this study, all samples were synthesized by the hydrothermal method at 160 °C for 6 h. The materials obtained were structurally characterized by X-ray diffraction (XRD) and structural Rietveld refinement, Raman spectroscopy, and infrared spectroscopy (FTIR), confirming the presence of all crystallographic planes and bands associated with active modes for the pure hexagonal phase (h-MoO3) when the solution's concentration was 0.6 mol L-1 of nitric acid. For concentrations of 1.10, 1.60, and 2.10 mol L-1, the presence of crystallographic planes and active modes associated with the formation of mixtures of molybdenum oxide polymorphs was confirmed, in this case, the orthorhombic, monoclinic, and hexagonal phases. X-ray photoelectron spectroscopy reveals the occurrence of the states Mo4+, Mo5+, and Mo6+, which confirm the predominance of the acid Lewis sites, corroborating the analysis by adsorption of pyridine followed by characterization by infrared spectroscopy. The images collected by scanning electron microscopy confirmed the information presented in the structural characterization, where microcrystals with hexagonal morphology were obtained for the MoO3_2.5 sample. In contrast, the MoO3_5, MoO3_7.5, and MoO3_10 samples exhibited hexagonal and rod-shaped microcrystals, where the latter morphology is characteristic of the orthorhombic phase. The catalytic tests carried out in the conversion of oleic acid into methyl oleate, using the synthesized samples as a heterogeneous catalyst, resulted in conversion percentages of 52.5, 58.6, 69.1, and 97.2% applying the samples MoO3_2.5, MoO3_5, MoO3_7.5, and MoO3_10, respectively. The optimization of the catalytic tests with the MoO3_10 sample revealed that the conversion of oleic acid into methyl oleate is a thermodynamically favorable process, with a variation in the Gibbs free energy between -67.3 kJ mol-1 and 83.4 kJ mol-1 as also, the energy value of activation of 24.6 kJ mol-1, for the temperature range from 80 to 140 °C, that is, from 353.15 to 413.15 K, respectively. Meanwhile, the catalyst reuse tests resulted in percentages greater than 85%, even after the ninth catalytic cycle. Therefore, the expressive catalytic performance of the mixture of h-MoO3 and α-MoO3 (MoO3_10) phases is confirmed, associated with the synergistic effect, mainly due to the increase in the surface area and available Lewis sites of these phases.