High-resolution X-ray Photoelectron Spectroscopy Research Articles

Reactivity of graphene-supported Co clusters

Graphene-supported Co clusters were investigated by high-resolution XPS, TPD and IRRAS using CO as a probe molecule. CO adsorption was observed at edge, on-top and bridge/hollow sites on the as-prepared clusters. Temperature-programmed XPS showed CO dissociation at T > 300 K. The CO desorption temperatures were determined by TPD measurements to be 260, 320 and 400 K for CObridge/hollow, COedge and COtop, respectively. The CO dissociation products were used to investigate the adsorption of CO on carbon and oxygen precovered Co clusters. Site blocking by these adatoms was found resulting in the absence of COedge (XPS and TPD) and a decrease of the CO adsorption capacity (XPS, TPD and IRRAS). Additionally, no CO dissociation was found on the precovered clusters concluding a blocking of the catalytically active sites which are the edge sites of the clusters.

The role of thickness on the structural and luminescence properties of Y2O3:Ho3+, Yb3+ upconversion films

The structural, surface, and upconversion (UC) luminescence properties of Y2O3:Ho3+,Yb3+ films grown by pulsed laser deposition, for different numbers of laser pulses, were studied. The crystallinity, surface, and UC luminescence properties of the thin films were found to be highly dependent on the number of laser pulses. The X-ray powder diffraction analysis revealed that Y2O3:Ho3+,Yb3+ films were formed in a cubic structure phase with an Ia 3¯\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\overline{3 }$$\\end{document} space group. The thicknesses of the films were estimated by using cross-sectional scanning electron microscopy, depth profiles using X-ray photoelectron spectroscopy (XPS), and the Swanepoel method. The high-resolution XPS was used to determine the chemical composition and oxidation states of the prepared films. The UC emissions were observed at 538, 550, 666, and 756 nm, assigned to the 5F4 → 5I8, 5S2 → 5I8, 5F5 → 5I8, and 5S2 → 5I7 transitions of the Ho3+ ions. The power dependence measurements confirmed the involvement of a two-photon process in the UC process. The color purity estimated from the Commission International de I’Eclairage coordinates confirmed strong green UC emission. The results suggested that the Y2O3:Ho3+,Yb3+ UC transparent films are good candidates for various applications, including solar cell applications.

Study on Catalytic Performance in CO2 Hydrogenation to Methanol over Au–Cu/C3N4 Catalysts

In this paper, Au and Cu nanoparticles were successfully loaded onto porous g-C3N4 material through a hydrothermal synthesis method. By adjusting the proportion of Cu, Au-5%Cu/C3N4, Au-10%Cu/C3N4, and Au-15%Cu/C3N4, catalysts were prepared and used for the catalytic reduction of CO2 to methanol. Characterization analysis using high-resolution XPS spectra showed that with an increase in the doping amount of Cu, the electron cloud density on the Cu surface initially increased and then decreased. Electrons from Au atoms transferred to Cu atoms, leading to the accumulation of a more negative charge on the Cu surface, promoting the adsorption of partially positively charged C in CO2, which is more beneficial for catalyzing CO2. Among them, Au-10%Cu/C3N4 exhibited good reducibility and strong basic sites, as demonstrated by H2-TPR and CO2-TPD, with the conversion rates for CO2, methanol yield, and methanol selectivity being 11.58%, 41.29 g·kg−1·h−1 (0.39 μmol·g−1s−1), and 59.77%, respectively.

Effect of temperature on the stability and performance of III-nitride HEMT magnetic field sensors

The study aimed to investigate the underlying physics limiting the temperature stability and performance of non-surface passivated Al0.34Ga0.66N/GaN Hall effect sensors, including contacts, under atmospheric conditions. The results obtained from analyzing the microstructural evolution in the Al0.34Ga0.66N/GaN Hall sensor heterostructure were found to correlate with the electrical performance of the Hall effect sensor. High-resolution x-ray photoelectron spectroscopy studies revealed the signature of surface oxidation in the GaN cap layer, as well as a slight out-diffusion of “Al” from the AlGaN barrier layer. To prevent the formation of a bumpy surface morphology at the Ohmic contact, we investigated the impact of “Pt” top Ohmic contacts. The application of a top “Pt” contact stack resulted in a smooth Ohmic contact surface and provided evidence that the bumpy surface morphology in Au-based Ohmic contacts is due to the formation of an Al-Au viscous alloy during rapid thermal annealing. In the early stages of thermal aging, the small drop in contact resistivity stabilized with subsequent thermal aging past the initial 550 h at 200 °C. The outcome is that the Al0.34Ga0.66N/GaN Hall effect sensors, even without surface passivation, exhibited a stable response to applied magnetic fields with no sign of significant degradation after 2800 h of thermal aging at 200 °C under atmospheric conditions. This observed stability in the Hall sensor without surface passivation can be attributed to a self-imposed surface oxidation of the cap layer during the early stages of aging, which serves as a protective layer for the device during subsequent extended periods of thermal aging at 200 °C.

Benchmarking diamond surface preparation and fluorination via inductively coupled plasma-reactive ion etching

Diamond, renowned for its exceptional semiconducting properties, stands out as a promising material for high-performance power electronics, optics, quantum, and biosensing technologies. This study methodically investigates the optimization of polycrystalline diamond (PCD) substrate surfaces through Inductively Coupled Plasma Reactive Ion Etching (ICP-RIE). Various parameters, including gaseous species, flow rate, coil power, and bias power were tuned to understand their impact on surface morphology and chemistry. A thorough characterization, encompassing chemical, spectroscopic, and microscopic methods, shed light on the effects of different ICP-RIE conditions on surface properties. CF4/O2 plasma emerged as a viable treatment for achieving smooth PCD surfaces with minimal etch pit formation. Most notably, surface fluorination, a critical aspect of increasing chemical and thermal stability, was successfully accomplished using CF4, SF6, and other F-containing plasmas. The fluorine concentration and surface chemistry variations were studied, with high resolution X-ray Photoelectron Spectroscopy unveiling differences amongst the sp2 C phase, sp3 C phase, C–O, CO, and C–F bonds. Time-of-flight secondary Ion Mass Spectrometry (ToF-SIMS) and depth-profile analysis unveiled a consistent surface fluorination pattern with CF4/O2 treatment. Furthermore, contact angle measurements showcased heightened hydrophobicity. This study provides valuable insights into precise diamond surface engineering, important for the development of future diamond-based semiconductor technologies.

Mango Leaves (Mangifera indica)-Derived Highly Florescent Green Graphene Quantum Dot Nanoprobes for Enhanced On-Off Dual Detection of Cholesterol and Fe2+ Ions Based on Molecular Logic Operation.

In the present study, we have engineered a molecular logic gate system employing both Fe2+ ions and cholesterol as bioanalytes for innovative detection strategies. We utilized a green-synthesis method employing the mango leaves extract to create fluorescent graphene quantum dots termed "mGQDs". Through techniques like HR-TEM, i.e., high-resolution transmission electron microscopy, Raman spectroscopy, and XPS, i.e., X-ray photoelectron spectroscopy, the successful formation of mGQDs was confirmed. The photoluminescence (PL) characteristics of mGQDs were investigated for potential applications in metal ion detection, specifically Fe2+ traces in water, by using fluorescence techniques. Under 425 nm excitation, mGQDs exhibited emission bands at 495 and 677 nm in their PL spectrum. Fe2+-induced notable quenching of mGQDs' PL intensity decreased by 97% with 2.5 μM Fe2+ ions; however, adding 20 mM cholesterol resulted in a 92% recovery. Detection limits were established through a linear Stern-Volmer (S-V) plot at room temperature, yielding values of 4.07 μM for Fe2+ ions and 1.8 mM for cholesterol. Moreover, mGQDs demonstrated biocompatibility, aqueous solubility, and nontoxicity, facilitating the creation of a rapid nonenzymatic cholesterol detection method. Selectivity and detection studies underscored mGQDs' reliability in cholesterol level monitoring. Additionally, a molecular logic gate system employing Fe2+ metal ions and cholesterol as a bioanalyte was established for detection purposes. Overall, this research introduces an ecofriendly approach to craft mGQDs and highlights their effectiveness in detecting metal ions and cholesterol, suggesting their potential as versatile nanomaterials for diverse analytical and biomedical applications.

Photoluminescence and light absorption edges of Bi2O2CO3 regulated by pressure-induced oxygen vacancies

In this work, Bi2O2CO3 (BOC) was subjected to high-pressure treatment using a diamond anvil cell at pressures of 0, 4.2, and 25.6 GPa to improve the photocatalytic performance. High-resolution transmission electron microscopy and X-ray photoelectron spectroscopy were employed for in-depth analysis. The results indicated that after treatment at 25.6 GPa, oxygen vacancies were induced in the powder, and defect energy levels were formed within the band gap of the BOC, thereby expanding its absorption of visible light. The light absorption edge shifted from 377 nm to 562 nm, which have enhanced the ability of separating photogenerated electron-hole pairs. This study demonstrates that high-pressure treatment is beneficial for improving the photocatalytic performance of Bi2O2CO3.

The heterointerface characterization of BaF2 or MgF2 on the hydrogenated diamond by X-ray photoelectron spectroscopy

Group-II fluorides (BaF2 and MgF2) insulators are deposited on hydrogenated (C–H) diamonds by E-beam evaporator at room temperature. The bandgaps, chemical bonds and band offsets of fluorides are investigated by the high-resolution X-ray photoelectron spectroscopy (XPS) measurements. The XPS results show bandgap energies of 9.4 ± 0.2 eV for BaF2 and 9.7 ± 0.2 eV for MgF2 by F 1s energy loss spectra. The valence band offsets (ΔEV's) of BaF2/MgF2 on the C–H diamond are determined as 5.2 ± 0.2 and 4.8 ± 0.2 eV, respectively. There are both type II energy band configuration for BaF2 and MgF2 on the C–H diamond with conduction band offsets of 1.3 ± 0.2 eV and 0.6 ± 0.2 eV, respectively. The relatively oxygen-weak or oxygen-free fluoride/C–H diamond interface and large ΔEV suggest that fluorides are an excellent gate dielectric for the C–H diamond field-effect transistors with high hole mobility and low gate leakage.

Direct Photocatalytic Methane Oxidation to Formaldehyde by N Doping Co-Decorated Mixed Crystal TiO2.

In this paper, N-doped TiO2 mixed crystals are prepared via direct calcination of TiN for highly selective oxidation of CH4 to HCHO at room temperature. The structures of the prepared TiO2 samples are characterized to be N-doped TiO2 of anatase and rutile mixed crystals. The crystal structures of TiO2 samples are determined by XRD spectra and Raman spectra, while N doping is demonstrated by TEM mapping, ONH inorganic element analysis, and high-resolution XPS results. Significantly, the production rate of HCHO is as high as 23.5 mmol·g-1·h-1 with a selectivity over 90%. Mechanism studies reveal that H2O is the main oxygen source and acts through the formation of ·OH. DFT calculations indicate that the construction of a mixed crystal structure and N-doping modification mainly act by increasing the adsorption capacity of H2O. An efficient photocatalyst was prepared by us to convert CH4 to HCHO with high yield and selectivity, greatly promoting the development of the photocatalytic CH4 conversion study.

Unveiling Enhanced PEC Water Oxidation: Morphology Tuning and Interfacial Phase Change in α-Fe2O3@K-OMS-2 Branched Core-Shell Nanoarrays.

A simple fabrication method that involves two steps of hydrothermal reaction has been demonstrated for the growth of α-Fe2O3@K-OMS-2 branched core-shell nanoarrays. Different reactant concentrations in the shell-forming step led to different morphologies in the resultant composites, denoted as 0.25 OC, 0.5 OC, and 1.0 OC. Both 0.25 OC and 0.5 OC formed perfect branched core-shell structures, with 0.5 OC possessing longer branches, which were observed by SEM and TEM. The core K-OMS-2 and shell α-Fe2O3 were confirmed by grazing incidence X-ray diffraction (GIXRD), EDS mapping, and atomic alignment from high-resolution STEM images. Further investigation with high-resolution HAADF-STEM, EELS, and XPS indicated the existence of an ultrathin layer of Mn3O4 sandwiched at the interface. All composite materials offered greatly enhanced photocurrent density at 1.23 VRHE, compared to the pristine Fe2O3 photoanode (0.33 mA/cm2), and sample 0.5 OC showed the highest photocurrent density of 2.81 mA/cm2. Photoelectrochemical (PEC) performance was evaluated for the samples by conducting linear sweep voltammetry (LSV), applied bias photo-to-current efficiency (ABPE), electrochemical impedance spectroscopy (EIS), incident-photo-to-current efficiency (IPCE), transient photocurrent responses, and stability tests. The charge separation and transfer efficiencies, together with the electrochemically active surface area, were also investigated. The significant enhancement in sample 0.5 OC is ascribed to the synergetic effect brought by the longer branches in the core-shell structure, the conductive K-OMS-2 core, and the formation of the Mn3O4 thin layer formed between the core and shell.

A novel MXene-bridged Z-scheme ZnO@Nb2CTx MXene@carbon nitride nanosheets photocatalyst for efficient enrofloxacin degradation

A Z-scheme photocatalyst, ZnO@Nb2CTx MXene@carbon nitride nanosheets (ZNC), is synthesized by the hydrothermal and electrostatic self-assembly strategy. The degradation test shows that ZNC photocatalyst has an enhanced photocatalytic efficiency of Enrofloxacin (ENR) degradation under visible light irradiation. The ENR removing rate has reached 98.2 % after 40 min light irradiation and has a degradation rate of 0.0961 min−1, which is 4.78 times higher than pure ZnO and 3.987 times higher than CNNS. Besides, a possible ENR degradation pathway was studied via LC-MS method. Furthermore, in-situ high resolution XPS spectroscopy and DFT calculation confirmed the direction of electron flow in the ZNC photocatalyst, highlighting that its improved degradation efficiency primarily stems from the introduction of the MXene electron transport layer, which promotes efficient charge transfer and separation of electron-hole pair. This study provides a guidance to design highly efficient Z-scheme photocatalyst for ENR degradation.

Effective adsorption of fluorescent congo red azo dye from aqueous solution by green synthesized nanosphere ZnO/CuO composite using propolis as bee byproduct extract.

The indirect dumping of massive volumes of toxic dyes into water has seriously affected the ecosystem. Owing to the many applications of the designed nanomaterials in the manufacturing process, there is a lot of research interest in synthesizing nanomaterials using green processes. In this research, the byproduct of bee was employed to synthesize nanoparticles (NPs) of ZnO, CuO, and biosynthesized ZnO/CuO (BZC) nanocomposite via utilizing a green and simple approach. To validate the effective fabrication of BZC nanocomposite, various characterization measurements were applied. FTIR analysis identified the functional groups in charge of producing nanoparticles and nanocomposites. Moreover, the existence of ZnO and CuO XRD peaks suggests that the nanocomposites were successfully biosynthesized. The high-resolution XPS spectrum of the BZC nanocomposite's Zn2p3, Cu2p3, and O1s were observed. Our findings indicate the successful engineering of the prepared nanomaterials and BZC nanocomposite. Our findings indicate the successful engineering of the prepared nanomaterials and BZC nanocomposite. For Congo red (CR) fluorescent stain azo dye elimination in water, all adsorption parameters were examined at room temperature. Moreover, the adsorption experiments revealed the removal capacity for uptake CR dye using BZC nanocomposite (90.14mgg-1). Our results show that the BZC nanocomposite exhibited high removal capability for the adsorption of CR dye. The nanosphere adsorbent offered a simple, low-cost, and green approach for water purification and industrial wastewater control.

H-BN in the making: The surface chemistry of borazine on Rh(111)

Borazine is a well-established precursor molecule for the growth of hexagonal boron nitride (h-BN) via chemical vapor deposition on metal substrates. To understand the formation of the h-BN/Rh(111) moiré from borazine on a molecular level, we investigated the low-temperature adsorption and thermally induced on-surface reaction of borazine on Rh(111) in situ using synchrotron radiation-based high-resolution x-ray photoelectron spectroscopy (XPS), temperature-programmed XPS, and near-edge x-ray absorption fine structure measurements. We find that borazine adsorbs mainly as an intact molecule and have identified a flat-lying adsorption geometry. Borazine multilayers are observed to desorb below 200 K. Starting at about 300 K, dehydrogenation of the remaining borazine and borazine fragments takes place, and disordered boron nitride starts to grow. Above 600 K, the formation of the h-BN sets in. Finally, at 1100 K, the conversion to h-BN is complete. The h-BN formed by deposition and post-annealing was compared to the h-BN grown by an established procedure, proving the successful preparation of the desired two-dimensional material.

Innovative synthesis technique for high-performance dielectric resonator antennas: laser-induced shockwave sintering of potassium sodium niobate (KNN)

This study explored the synthesis and sintering of potassium sodium niobate (KNN) nanoparticles, emphasizing morphology, crystal structure, and sintering methods. The as-synthesized KNN nanoparticles exhibited a spherical morphology below 200 nm. Solid state sintering (SSS) and laser-induced shockwave sintering (LISWS) were compared, with LISWS producing denser microstructures and improved grain growth. Raman spectroscopy and x-ray diffraction confirmed KNN perovskite structure, with LISWS demonstrating higher purity. High-resolution x-ray photoelectron spectroscopy spectra indicated increased binding energies in LISWS, reflecting enhanced density and crystallinity. Dielectric and loss tangent analyses showed temperature-dependent behavior, with LISWS-3 exhibiting superior properties. Antenna performance assessments revealed LISWS-3’s improved directivity and reduced sidelobe radiation compared to SSS, attributed to its denser microstructure. Overall, LISWS proved advantageous for enhancing KNN ceramics, particularly in antenna applications.

Combined experimental and first principles look into (Ce, Mo) doped BiVO4

Here we investigated the effects of Ce and Mo doping on hydrothermally synthesized bismuth vanadate BiVO4 nanoparticles (NPs). The existence of monoclinic scheelite and tetragonal zircon phases of NPs was validated from Rietveld refinement of the powdered X-ray diffraction, room temperature Raman, and Fourier-transform infrared spectroscopy. The co-doping of Bi and V sites with respective Ce and Mo dopants in a mixed tetragonal zircon and monoclinic scheelite phases of BiVO4 lattice was corroborated from high-resolution transmission electron microscopy and X-ray photoelectron spectroscopy. The photoluminescence measurements revealed enhancement of photo-generated carrier recombination in (Ce, Mo) co-doped BiVO4 NPs which may have hampered its photocatalytic efficiency in degrading the methylene blue dye. The simulations based on Hubbard U corrected density functional theory (DFT+U) suggest that Mo and Ce co-doping introduced deep impurity states which may have facilitated the photo-generated carrier recombination detrimental to photocatalytic performance. The UV-vis diffuse reflectance measurements provided evidence for the presence of these defect states. In summary, this work may have presented a comprehensive experimental analysis of (Ce, Mo) doped BiVO4 supported by DFT simulations.

BN nanosheets/aramid nanofibers with pearl layered structure towards highly thermal conductive composites

This work reports a composite film using (3-Aminopropyl)triethoxysilane-modified boron nitride nanosheets (BNNS) incorporated in the aramid nanofibers (ANF) network via sol–gel method. High-resolution TEM, SEM, XPS, and XRD outcomes confirmed the imitation pearl layered structure—BNNSs as thermal conductive fillers were layer-by-layer overlapped on ANF. The reasonable coordination between interfaces and fillers stimulated the thermal conductivity (35.4 W (m·k)-1) of composite film i.e., 338.43 % higher than that of ANF. The composite film exhibited good cyclic thermal stability, high tensile strength (65.9 MPa), and high volume resistivity (2.424 × 1015 Ω∙cm).

Effect of graphene oxide and carbon black on the thermoelectric performance of niobium doped strontium titanate

Strontium titanate-based ceramics are promising n-type thermoelectrics due to their low cost and high thermal and chemical stability. Here, SrTi0.85Nb0.15O3 was prepared with carbon additions of electrochemically produced graphene oxide (eGO) and commercially available carbon black (CB). Ceramic samples were sintered at 1700 K under a reducing atmosphere. XRD, HR-TEM and Raman spectra confirmed the matrix phase was cubic perovskite; there were no carbon residues. By incorporating graphene oxide, the electrical conductivity increased nine-fold to 2818 S cm−1 at 300 K as a result of enhanced carrier mobility. In contrast, the carbon black samples exhibited low density and a small average grain size of ∼1 μm. High-resolution X-ray photoelectron spectroscopy revealed the presence of a large number of ionised impurities in the carbon black samples, which significantly enhanced scattering effects; low thermal conductivities of 1.7 W m−1 K−1 were achieved at 873 K. The work reveals that eGO promotes charge transport in SrTiO3, while CB significantly suppresses phonon transport. Both effects are relevant to the development of other thermoelectrics.

Encapsulated cementite enhances catalytic performance of carbon nanotubes for oxygen reduction reaction

Nonprecious-metal-based materials show great potential to be highly efficient catalysts for oxygen reduction reaction (ORR). There is still room for improvement in the performances of nonprecious-metal-based catalysts for ORR. In this paper, we investigated the catalytic performances of N-doped carbon nanotubes (CNTs) with encapsulated cementite (Fe3C@CNT) for ORR. The encapsulation structure was confirmed by scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy analyses. The catalytic performances of Fe3C@CNT for ORR were investigated by cyclic voltammetry, linear sweep voltammetry, Tafel analysis, rotating disk electrode, and rotating ring-disk electrode tests. The results showed that both the onset potential and half-wave potential of Fe3C@CNT-catalyzed ORR were 60 mV higher than those of 20 wt% Pt/C catalyst. Fe3C@CNT catalyzed ORR mainly happened through a four-electron pathway. The long-time running stability of the Fe3C@CNT was also superior to that of the 20 wt% Pt/C catalyst. The eutectic layers between the CNTs and cementite enhanced the electron transfer from the inner-layer CNT to the surface-layer N-doped CNT. Calculations revealed that the iron and carbon in the cementite were in positive and negative electronic states, respectively. The encapsulated cementite promoted the formation of equipotential circles on the surface-layer CNT, which greatly enhanced the catalytic performance of the Fe3C@CNT for ORR. N-doped CNTs with encapsulated cementite show great potential to be high-performance catalysts for ORR.

Self-assembled graphene oxide thin films deposited by atmospheric pressure plasma and their hydrogen thermal reduction

This work uses an atmosphere-pressure plasma jet to obtain thin, homogeneous graphene oxide coatings. The films consisted of self-assembled graphene oxide (GO) layers, which were reduced by heat treatment under a reductive hydrogen atmosphere to obtain a reduced graphene oxide film. The electrochemical and photoelectrochemical analyses show that electrical conductivity increases after the reduction process; meanwhile, this process eliminates the p-type photoactivity of the graphene oxide film. The reduced graphene oxide X-ray diffraction pattern revealed the elimination of the signal at 2θ = 11° initially found in the graphene oxide film. The C1s and O1s high-resolution XPS analyses of the reduced graphene oxide film reveal a pronounced increase in the graphitic-like carbon (sp2), whereas a decrease in the organic-like carbon (sp3) and oxygenated species, such as C-OH, C-O-C, CO, and OCOH, initially found in the graphene oxide film.

Effects of polyoxymethylene dimethyl ethers (PODEn) on soot characteristics in isooctane inverse diffusion flames

Polyoxymethylene dimethyl ethers (PODEn, n = 1–3) such as dimethoxymethane (DMM) and PODE3 are considered highly promising alternative fuels due to their lack of C–C bonds and significant oxygen contents. Particularly, PODE3-blends with diesel have been proven to substantially reduce soot emissions and fuel consumption rates under optimized engine conditions, although the impact on soot nanostructure properties remains unclear. This study explored the effects of DMM and PODE3 on soot characteristics in isooctane (i-octane) inverse diffusion flames, focusing on soot morphology, soot nanostructure, soot nanocrystallite, and soot spectral features. To compare soot particles behavior, DMM and PODE3 blended as the isooctane substitute (by 20% and 40% volumetric fractions) were examined with various diagnostic techniques, including high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), Raman spectroscopy, and X-ray photoelectron spectroscopy (XPS).The results showed that DMM and PODE3 contributed to a reduction in sooting tendency from i-octane flames, whereas the average soot mass decreased significantly as the PODE3 ratio increased, consistent with a higher oxygen concentration. Therefore, 20% PODE3/i-octane exhibited growing disorganized arrangements of soot particles with shorter fringes, smaller crystallite sizes, and a relatively lower degree of graphitization than 20% and 40% DMM additions. However, XPS analysis indicated that soot produced from PODE3/i-octane mixtures had less oxygen atoms because PODE3 has multiple –CH2O- chain groups that can convert oxygen into carbon monoxide with little soot production. Moreover, HRTEM, XRD, and Raman spectra analyses of 40% PODE3-doped flames confirmed an exceptional correlation with turbostratic soot structure, as manifested by the shortest fringe length, longest fringe tortuosity, more amorphous soot with the smallest crystallite dimensions, and least degree of graphitization.