High-resolution X-ray Diffraction Research Articles

Low loss ridge waveguides on the hybrid single crystalline silicon and lithium niobate thin films

The hybridization of silicon (Si) thin film and lithium niobate (LN) thin film with remarkable properties, including the excellent optical properties of LN, excellent electrical properties and mature processing advantages of Si, can provide an important material platform for integrated photonic applications. In this work, a 4-inch single crystalline Si thin film wafer was prepared using wafer bonding, grinding and polishing techniques on LN thin film substrate. The films were characterized by using high-resolution transmission electron microscopy (HRTEM). The interplanar spacings and strain of Si film were calculated by analysis of high-resolution X-ray diffraction (HRXRD). Si ridge straight waveguides were fabricated on the hybrid thin films, and the transmission loss was 1.2dB/cm. The near-field mode distribution of the waveguide was investigated by combining FDTD (Finite-Difference Time-Domain) simulation and end coupling measurement.

Pinpointing lattice-matched conditions for wurtzite ScxAl1−xN/GaN heterostructures with x-ray reciprocal space analysis

Using comprehensive x-ray reciprocal space mapping, we establish the precise lattice-matching composition for wurtzite ScxAl1−xN layers on (0001) GaN to be x = 0.14 ± 0.01. 100 nm thick ScxAl1−xN films (x = 0.09–0.19) were grown in small composition increments on c-plane GaN templates by plasma-assisted molecular beam epitaxy. The alloy composition was estimated from the fit of the (0002) x-ray peak positions, assuming the c-lattice parameter of ScAlN films coherently strained on GaN increases linearly with Sc-content determined independently by Rutherford backscattering spectrometry [Dzuba et al., J. Appl. Phys. 132, 175701 (2022)]. Reciprocal space maps obtained from high-resolution x-ray diffraction measurements of the (101¯5) reflection reveal that ScxAl1−xN films with x = 0.14 ± 0.01 are coherently strained with the GaN substrate, while the other compositions show evidence of relaxation. The in-plane lattice-matching with GaN is further confirmed for a 300 nm thick Sc0.14Al0.86N layer. The full-width-at-half-maximum of the (0002) reflection rocking curve for this Sc0.14Al0.86N film is 106 arc sec and corresponds to the lowest value reported in the literature for wurtzite ScAlN films.

Influence of low-temperature cap layer thickness on the structure and luminescence of InGaN/GaN multiple quantum wells

In order to effectively regulate the luminescence performance of MQW and enhance its optical quality, it is crucial to investigate the InGaN/GaN MQW's structure and luminescence properties. In this study the focus is how they are affected by low-temperature cap (LT-cap) layer's thickness which is grown above each InGaN well layer during growth process of InGaN/GaN multiple quantum well (MQW) samples in MOCVD system. This was achieved by analyzing high resolution X-ray diffraction (HRXRD) spectra, electroluminescence (EL) spectra, temperature-dependent photoluminescence (TDPL) spectra, and micro-area fluorescence imaging of these samples. The results show that changes in LT-cap layer's thickness even have no significant impact on some structural parameters of MQW, such as the thickness of the well layer, but have an influence on the In component of the well layer. Due to the existence of LT-cap layer, dissociation of InGaN can be effectually reduced. In addition, the augmentation of LT-cap layer's thickness will make polarization effect of the QW sample more remarkable, so that the blue shift of the EL peak with the augmentation of current injection increases. The change of LT-cap layer's thickness will also influence distribution of the tail states of the quantum wells, which leads to a different localization states for injected carriers. As LT-cap layer becomes getting thicker, the material's internal quantum efficiency (IQE) tends to decrease, which may result from an increase in non-radiative recombination centers.

Molecular structure and evolution mechanism of shale kerogen: Insights from thermal simulation and spectroscopic analysis

During thermal evolution, the kerogen in shale formation undergoes significant chemical, structural and compositional changes, continuously influencing the shale storage capacity, hydrocarbon generation potential, and gas occurrence state. This study systematically examines the chemical structural changes during the thermal evolution of Longmaxi shale kerogen using hydrothermal laboratory experiments from 420 to 850 °C. Additionally, a range of characterization techniques, including Fourier Transform Infrared (FTIR) spectroscopy, Raman spectroscopy, High-Resolution Transmission Electron Microscopy (HRTEM), X-ray Diffraction (XRD), and Solid-state 13C Nuclear Magnetic Resonance (13C NMR), were employed to systematically investigate the kerogen structure and its evolution patterns. Results indicate that Longmaxi Formation kerogen comprises a large molecular carbon framework with aromatic structures, long-chain aliphatic components, and oxygen-containing functional groups. As thermal maturity reaches 2.6 %, the alignment of aromatic fringes gradually increased, with over 60 % aligning in the main direction. Throughout thermal evolution (1.9–3.2 %), fringes in the 5–10 Å range within aromatic structures peak at over 20.45 %, with fringes over 50 Å rapidly increasing from 3 % to over 15 %. Early in the thermal evolution, the long-chain aliphatic component of the kerogen decreases rapidly and part of the structure forms small aromatic rings through aromatisation. The mature to over-mature stage can be divided into three phases: 1) 1.7–2.4 % (loss of oxygen-containing functional groups), 2) 2.4–3.5 % (formation of larger aromatic structures via condensation reactions), 3) over 3.5 % (continued aggregation of aromatic rings, resulting in an increase in the length of aromatic fringes). At a macroscopic level, this induces changes in kerogen pore structure and carbonization features. This study thus provides new insights into the thermal evolution of shale kerogen, which in turn improve understanding of shale reservoirs for hydrocarbon exploitation.

Enhancement of superconductivity and structural phase transitions under pressure in FeTe0.89S0.11

The ternary iron chalcogenide, FeTe0.89S0.11 is a prominent member of the family of Fe-based superconductors with an ambient pressure Tc of around 8 K and a simple structure formed by layers of edge-sharing distorted tetrahedra separated by a van der Waals gap. Upon compression to 6 GPa, the Tc increases monotonically to 11 K. The superconductivity disappeared at about 6 GPa which was correlated to a softening of a Raman mode. High-resolution synchrotron X-ray diffraction shows that the FeTe0.89S0.11 started to transform from the monoclinic phase described by space group Cm to a disordered triclinic phase described by space group P1 at around 10 GPa (theoretical) - 14 GPa (experimental). Due to the phase transition the studied material transforms from a layered compound to a polymer, which is accompanied by a volume collapse of 4.65 %, indicating a discontinuous first-order phase transition. The disappearance of Raman modes, along with pressure independent resistivity, and ab initio calculations results support the structural and electronics phase transition. According to our results Fe(Te,S) may be useful for future high-field power applications being formed of relatively inexpensive and nontoxic elements.

Synchrotron-based x-ray diffraction analysis of energetic ion-induced strain in GaAs and 4H-SiC

Strain engineering using ion beams is a current topic of research interest in semiconductor materials. Synchrotron-based high-resolution x-ray diffraction has been utilized for strain-depth analysis in GaAs irradiated with 300 keV Ar and 4H-SiC and GaAs irradiated with 100 MeV Ag ions. The direct displacement-related defect formation, anticipated from the elastic energy loss of Ar ions, can well explain the irradiation-induced strain depth profiles. The maximum strain in GaAs is evaluated to be 0.88% after Ar irradiation. The unique energy loss depth profile of 100 MeV Ag (swift heavy ions; SHIs) and resistance of pristine 4H-SiC and GaAs to form amorphous/highly disordered ion tracks by ionization energy loss of monatomic ions allow us to examine strain buildup due to the concentrated displacement damage by the elastic energy loss near the end of ion range (∼12 μm). Interestingly, for the case of SHIs, the strain-depth evolution requires consideration of recovery by ionization energy loss component in addition to the elastic displacement damage. For GaAs, strain builds up throughout the ion range, and the maximum strain increases and then saturates at 0.37% above an ion fluence of 3×1013 Ag/cm2. For 4H-SiC, the maximum strain reaches 4.6% and then starts to recover for fluences above 1×1013 Ag/cm2. Finally, the contribution of irradiation defects and the purely mechanical contribution to the total strain have been considered to understand the response of different compounds to ion irradiation.

Insights into impact of shock wave on structural, optical and surface characteristics of ammonium pentaborate tetrahydrate single crystal

In this study, we are emphasizing on growth of bulk size optically transparent single crystals of ammonium pentaborate tetrahydrate (APB) using the slow evaporation solution technique at room temperature. Initially, crystalline phase of the compound was confirmed through the X-ray diffraction technique. Thereafter, APB has been analysed systematically for its crystallographic structural stability in such a way that its structure has been examined periodically at two shock wave (SW) loaded conditions using XRD measurements. Further, our research contains a comprehensive knowledge about effect of shock wave on rocking curve of APB single crystal measured through high resolution XRD measurement system and the changes in crystalline perfection due to shock wave was analysed. Also, modifications in optical properties were studied due to impact of shock waves. The transmittance was checked through UV–visible spectroscopy and the changes in optical band gap were examined. The defects generated in the APB crystal after every two shocks i.e., shockwave - sample interaction was scrutinized by photoluminescence spectroscopy and surface morphology studies in detail.

Effects of Fe substitution for Mn on structural, magnetic and magnetocaloric properties of TbMn2-xFexSi2

The structural and magnetic properties of TbMn2-xFexSi2 compounds (x = 0.0–0.4) have been investigated in details by high-resolution synchrotron x-ray and neutron powder diffraction, specific heat, and dc magnetization measurements. The replacement of Fe for Mn in TbMn2-xFexSi2 does not change the crystal structure but leads to a significant contraction of the unit cell (dV/dx ∼ - 6 Å3) and modification of three magnetic phase transition temperatures – the Curie temperatures Tc1, Tc2 and the Néel temperature TN. For example, the Tc1, Tc2 and TN values of TbMn2Si2 decrease from Tc1 = 50 K, Tc2 = 64 K and TN = 500 K to Tc1 = 27 K, Tc2 = 37 K and TN = 440 K for TbMn1.6Fe0.4Si2. Detailed neutron diffraction investigations have allowed us to determine the magnetic structures and construct the magnetic phase diagram as well as confirm the presence of magnetoelastic coupling effects. The significantly different responses of Tc1 and Tc2 to applied magnetic fields (e.g. dTc1/dB = 0.52 K/T and dTc2/dB = 4.7 K/T for TbMn1.6Fe0.4Si2), leads to expansion of the temperature region (ΔT = Tc2- Tc1) for the canted ferromagnetic state Fmc-ii between Tc1 and Tc2. In the case of TbMn1.6Fe0.4Si2, ΔT increases from ΔT = 9 K for applied magnetic field B = 0.2 T to ΔT = 36 K for B = 6 T, resulting in plateau-like behaviour of magnetic entropy change and enhances the relative cooling power (RCP) in this system. Under a change of magnetic field of 0 T – 5 T, the maximum value of the magnetic entropy changes -ΔSmax and adiabatic temperature change, ΔTad are derived to be -ΔSmax = 13.1 J/kg K and ΔTad = 8.4 K with the RCP = 411 J/kg for x=0.4 sample. The plateau-like magnetocaloric effect and relatively large RCP make these materials potentially suitable for application in cryogenic magnetic refrigeration.

A luminescent metal–organic framework composite as a turn-on sensor for the selective determination of monosodium glutamate in instant noodles

This work reports the development and application of a new fluorescent nanoprobe sensor depending on using luminescent metal organic framework (LMOF). The developed sensor composed of hybridized Ca 1,3,5-benzenetricarboxylic acid metal organic framework with microcrystalline cellulose (Ca-BTC/MCC MOF) as a fluorescent probe for the determination of the monosodium glutamate (MSG), a non-chromophoric food additive. The developed sensor was characterized using a high-resolution scanning electron microscope (HR-SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The Ca-BTC/MCC MOF hybrid, examined under the HR-SEM, showed morphological features different from the MCC and the Ca-BTC MOF. The diffraction patterns of Ca-BTC/MCC composites clearly displayed the characteristic Ca-BTC MOF diffraction bands, indicating that MCC was successfully incorporated in the formation of crystalline MOF hybrids. The FTIR spectra show the bands of MCC, as well as the bands of Ca-BTC MOFs. The prepared nanoprobe was successfully applied as a sensitive sensor for the determination of MSG in food sample. The method was validated following the International ICH (Q2)R2 guidelines in terms of precision, trueness and other main analytical figures of merit, comprised the green profile and practicability metrics. A wide linearity range was achieved (5–50 µg/mL) with good correlation coefficient (R2 ≥ 0.9993). The recoveries (%) were found in the range of 100.0 to 101.5 and the RSDs (%) were in the range of 0.1 to 0.9 %.These results show that the developed nanoprobe was selective, and highly accurate to determine this important food additive in the seasonings of instant noodles, also showing a reduced environmental impact based on the metrics currently accepted for the evaluation of the green profile and practicability.

Identifying orientation-dependent optical properties of single-crystalline β-Ga2O3 films

We explore the effect of crystallographic anisotropy on the optical properties of high-quality β-Ga2O3 thin films by conducting experimental measurements and theoretical simulations. High resolution x-ray diffraction measurements confirm the high-quality and the single crystalline quality, ruling out the effect of defects for all films. Raman spectra reveal the presence of anisotropy, as evident from a stronger Bg(2) mode related to GaIO4 chain libration in (100) orientation. Conversely, a stronger Ag(10) mode corresponding to tetrahedral bonds is evident in the (010) orientation, while it is suppressed in the (100) orientation. Low-temperature photoluminescence spectra indicate the presence of intrinsic impurity-related emissions in the ultraviolet and blue regions for all films. An anisotropic bandgap is observed, wherein the lowest bandgap value is related to the (010) oriented sample. Spectroscopic ellipsometry measurements confirm different refractive indices and extinction coefficient values depending on crystallographic orientation, which are in good agreement with the theoretical values obtained by density functional theory, confirming the anisotropic characteristics. The theoretical calculations of charge density show that the strength of covalent bonding depends on the β-Ga2O3 orientation, while experimental findings demonstrate that as the covalent bonding character increases, the film bandgap and the refractive index decrease. The anisotropy of β-Ga2O3 with respect to the crystal orientation leads to variations in the extinction coefficient, refractive index, and bandgap energy.

Episodic hydrothermal supply and microbial anaerobic Fe(II) oxidation in early Archean ocean: Insights from precursor mineral compositions of the 3.46 Ga Marble Bar Chert, Pilbara Craton, Western Australia

The 3.46 Ga Marble Bar Chert (MBC) from the Pilbara Craton in Western Australia is known as the oldest chert on Earth. The origin of its Fe minerals was investigated to decipher the geochemistry and redox conditions of the early Archean ocean, as well as to explore the possible microbial contribution to the earliest sedimentary processes on Earth. However, the composition of the precursor minerals in the MBC remains poorly understood, giving rise to controversies on its genesis. Here we performed high-resolution petrographic, laser Raman, Mössbauer, X-ray diffraction, and Mn K-edge X-ray absorption near edge structure spectroscopic studies on two typical types of finely laminated MBC, grey-black chert and red chert. The grey-black chert contains considerable amounts of siderite, carbonaceous materials, and minor phyllosilicates and hematite. By contrast, the red chert contains high hematite and silicates, minor siderite and rare carbonaceous materials. Microcrystals in the cores of chert polyhedral are among the earliest mineral phases without signs of alterations, recrystallisation, erosion or replacement histories. Ferrihydrite, greenalite, siderite, and green rust are possible precursors of Fe-bearing minerals in the MBC. Their respective proportion in each lamina was regulated by pH, Fe(II)-oxidation rate, DIC, and Fe(II) content in the seawater. Approximately half Fe in the MBC primary minerals existed as Fe(III), indicating the existence of indigenous Fe(II)-oxidation in the Paleoarchean seawater. The element Mn in the MBC is primarily Mn(II) coordinated with O, suggesting a reduced depositional environment and hence implying the involvement of anaerobic microbial Fe(II)-oxidation in the formation of the MBC. Collectively, the grey-black laminae with abundant carbonaceous materials reflect limited Fe(II)-oxidation and increased dissolved inorganic carbon content likely due to enhanced hydrothermal CO2 supply, while the red laminae with considerable hematite represent substantial Fe(III)-supply due to rapid indigenous anaerobic Fe(II)-oxidation.

The enhanced GaN deposition on highly N-incorporated diamond substrate

As typical impurities in diamonds, the incorporated nitrogen (N) atoms could alleviate the wetting issues of GaN deposition on diamonds. Therefore, GaN was deposited on the N-incorporated diamond substrate. Through X-ray diffraction (XRD) characterization, the enhanced AlN was observed on the highly-N incorporated diamond substrate. Moreover, GaN morphology on N-incorporated diamond was greatly enhanced, showcasing superior film quality, which would be further confirmed by the Raman and photoluminescence spectra. Notably, high-resolution XRD characterization unveiled a much narrower rocking curve for GaN films on N-incorporated diamond substrates, with a full width at half maximum of 2714 arcsec, compared to 7560 arcsec on N-free diamond substrates. In conclusion, utilizing N-incorporated diamond substrates is a practical approach for GaN-on-diamond deposition.

Subsurface damage evolution of β-Ga2O3 (010) substrates during lapping and chemical mechanical polishing

For semiconductor single crystal substrates, subsurface damage (SSD) is an important factor for device failure. For β-Ga2O3 with two cleavage planes, the SSD is the key issue that needs to be addressed. In this work, β-Ga2O3 (010) substrates were lapped and polished precisely. The formation and evolution mechanisms of SSD were analyzed by cross-section transmission electron microscopy and wet chemical etching techniques. The linear distribution of scratches was found on the substrates after lapping. After chemical mechanical polishing (CMP), the surface scratches were eliminated. However, the SSD layer may still exist under the surface. Chemical etching was developed to identify the "invisible damage" to the CMP-finished (010) substrate. The SSD including nanocrystalline, tilt boundary, twist boundary, and high-density dislocations in β-Ga2O3 was first reported. Distinctively, there was no slip occurrence in the SSD of the (010) plane different from the (100) and (001) planes. The Schmid factor of multiple slip systems was calculated to analyze the cause of no slip on the subsurface. The formation mechanism of SSD was believed that when the slip system could not be activated, the stress was released through rotation and distortion of the crystal plane. The accumulation of grain boundary dislocations at twist grain boundary junctions provided a driving force for the formation of nanovoids. The relationship of substrate damage evolution and crystal strain with different machining parameters was established by high-resolution X-ray diffraction and Raman spectra. A non-damaging β-Ga2O3 (010) substrate with a surface roughness of less than 0.2 nm was obtained by the optimized CMP process. The research results had guiding significance for damage control of β-Ga2O3 and other brittle crystals in ultra-precision machining.

Effect of Mo on the coherent interface features of γ′-phase strengthened Co-based superalloys

Molybdenum (Mo) addition was investigated for its influence on the interfacial characteristics of γ′-phase strengthened Co-based superalloys with γ/γ′ dual phases. Advanced characterization techniques, including scanning transmission electron microscopy (STEM), atom probe tomography (APT), and high-resolution X-ray diffraction (HR-XRD), were employed for this purpose. Mo addition was found to increase the compositional and structural widths of the γ/γ′ interface. This was accompanied by segregation of Mo and Co at the interface, attributed to the reduction of interfacial energy. Additionally, Mo addition led to a decrease in the lattice misfit between the γ-matrix and γ′-phases. Those results enhanced interface stability, contributing to improved high-temperature stability. This study offers valuable insights into the mechanisms of alloying and the microstructural stability of Co-based superalloys.

Holmium-doped TbVO4 as a highly potential magneto-optical crystal for Faraday isolator

Tb1-xHoxVO4 (THV) magneto-optical crystal with diameter of 27 mm and length of 40 mm was grown by the Czochralski (Cz) technique for the first time. The structural perfection of THV crystal was studied by the high-resolution X-ray diffraction rocking curve measurement, proving the high crystallinity quality of THV. THV shows high transmittance of greater than 75 % within the wavelength range of 665–1600 nm. The Verdet constants of THV at 532, 633 and 1064 nm are 370, 226 and 56 rad·m−1T−1, 40 %–95 % higher than these of commercial TGG crystal. Additionally, THV exhibits lower absorption coefficient (0.05 cm−1), higher magneto-optical figure of merit (175 deg/dB) and extinction ratio (43 dB) at 1064 nm compared with TGG. Evaluation of thermal performance and laser-induced damage threshold of THV were also made to promote the potential application in high-power optical isolators.

Optical, Structural, and Synchrotron X-ray Absorption Studies for GaN Thin Films Grown on Si by Molecular Beam Epitaxy.

GaN on Si plays an important role in the integration and promotion of GaN-based wide-gap materials with Si-based integrated circuits (IC) technology. A series of GaN film materials were grown on Si (111) substrate using a unique plasma assistant molecular beam epitaxy (PA-MBE) technology and investigated using multiple characterization techniques of Nomarski microscopy (NM), high-resolution X-ray diffraction (HR-XRD), variable angular spectroscopic ellipsometry (VASE), Raman scattering, photoluminescence (PL), and synchrotron radiation (SR) near-edge X-ray absorption fine structure (NEXAFS) spectroscopy. NM confirmed crack-free wurtzite (w-) GaN thin films in a large range of 180-1500 nm. XRD identified the w- single crystalline structure for these GaN films with the orientation along the c-axis in the normal growth direction. An optimized 700 °C growth temperature, plus other corresponding parameters, was obtained for the PA-MBE growth of GaN on Si, exhibiting strong PL emission, narrow/strong Raman phonon modes, XRD w-GaN peaks, and high crystalline perfection. VASE studies identified this set of MBE-grown GaN/Si as having very low Urbach energy of about 18 meV. UV (325 nm)-excited Raman spectra of GaN/Si samples exhibited the GaN E2(low) and E2(high) phonon modes clearly without Raman features from the Si substrate, overcoming the difficulties from visible (532 nm) Raman measurements with strong Si Raman features overwhelming the GaN signals. The combined UV excitation Raman-PL spectra revealed multiple LO phonons spread over the GaN fundamental band edge emission PL band due to the outgoing resonance effect. Calculation of the UV Raman spectra determined the carrier concentrations with excellent values. Angular-dependent NEXAFS on Ga K-edge revealed the significant anisotropy of the conduction band of w-GaN and identified the NEXAFS resonances corresponding to different final states in the hexagonal GaN films on Si. Comparative GaN material properties are investigated in depth.

Growth of AlGaN alloys with ∼ 90 % AlN mole fraction by plasma-assisted molecular beam epitaxy: Indication of phase-segregation effects

AlGaN alloys with very high AlN mole fraction (∼90 %) were grown by plasma-assisted molecular beam epitaxy (PA-MBE) and their alloy properties were investigated by high-resolution X-ray diffraction (HR-XRD) measurements. Growth was carried out employing a series of group III/V ratios and for samples grown under a high group-III regime, phase-segregation in the alloy was evident from a characteristic splitting of the AlGaN (0002) peak in the HR-XRD pattern. With decreasing excess group-III conditions the separation of peak positions continuously reduced, till a single peak was observed. However, for samples where such splitting was absent, spontaneous superlattice peaks were seen at lower incident angles of the XRD patterns indicating the presence of long-range atomic ordering (LRAO). Thus, for AlGaN alloys with extremely high Al content, effects of phase-segregation, or of LRAO were observed, depending on the kinetics of growth. These results on phase-segregation effects are expected to promote the development of high-efficiency deep ultraviolet emitters for skin-safe germicidal action by mitigating the detrimental effect of dislocations and related non-radiative recombination centers through carrier localization processes at potential minima.

Dissecting of Atomic Morphology of Superfine Pulverized Coal Based on X-ray Pair Distribution Function

Resolving the atomic structure information of the aromatic layers in coal plays a crucial role in understanding the generation mechanisms of NOx during coal combustion and further reducing the formation of NOx from the source. This study reveals the distribution of X-ray diffraction bands of superfine pulverized coal using a high-resolution synchrotron radiation X-ray Diffraction (HRXRD) facility, discussing the distribution of atomic distances and atomic density in aromatic layers through pair distribution function (PDF) methods. Furthermore, the influences of mechanochemistry on the evolution of atomic morphology are focused on. The results show that the PDF of coal gradually stabilizes when r > 8 Å, showing the short-range order of graphite-like structure. Additionally, due to the limitations of scanning angle and X-ray energy, atomic distances in aromatic layers for coal are significantly greater than that of pure graphene. Enhanced mechanochemical effects make the peaks 1, 2, and 3 of coal PDF more similar to graphene's by condensing alkyl side chains into smaller, regular aromatic layers when the particle size decreases. With the enhancement of mechanochemical effects, coals with different metamorphic degrees exhibit different aromatic evolution patterns. The aromaticity of NMG coal first decreases and then increases, while the aromaticity of YQ coal shows the opposite trend. The results can provide deeper insights into the atomic structure of coal macromolecular, which can facilitate the advancement of novel ultra-low NOx combustion methods and support the construction of precise coal macromolecular models.

Radiation-Induced Synthesis and Superparamagnetic Properties of Ferrite Fe3O4 Nanoparticles.

Ultra-small magnetic Fe3O4 nanoparticles are successfully synthesized in basic solutions by using the radiolytic method of the partial reduction in FeIII in the presence of poly-acrylate (PA), or by using the coprecipitation method of FeIII and FeII salts in the presence of PA. The optical, structural, and magnetic properties of the nanoparticles were examined using UV-Vis absorption spectroscopy, high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), and SQUID magnetization measurements. The HRTEM and XRD analysis confirmed the formation of ultra-small magnetite nanoparticles in a spinel structure, with a smaller size for radiation-induced particles coated by PA (5.2 nm) than for coprecipitated PA-coated nanoparticles (11 nm). From magnetization measurements, it is shown that the nanoparticles are superparamagnetic at room temperature. The magnetization saturation value Ms = 50.1 A m2 kg-1 of radiation-induced nanoparticles at 60 kGy is higher than Ms = 18.2 A m2 kg-1 for coprecipitated nanoparticles. Both values are compared with nanoparticles coated with other stabilizers in the literature.

Optical constants and thickness determination of La[formula omitted]Sr[formula omitted]MnO3 thin films on Nb:SrTiO3 substrates by spectro-ellipsometry: Combination of optical and X-ray techniques

40 nm thick La2/3Sr1/3MnO3 (LSMO) thin films were epitaxially grown by Pulsed Laser Deposition (PLD) onto niobium doped SrTiO3 (Nb:STO) substrates, with different Nb concentration from 0.01%wt to 0.5%wt. The optical characterization of the heterostructures by spectroscopic ellipsometry enables us to extract the optical constants of the manganite heteroepitaxial layer at room temperature. Performing spectrophotometry in the same wavelength range brings a useful cross-validation of the extracted results. In addition, the thickness evaluation of the LSMO layer by spectro-ellipsometry is further validated by both High Resolution X-ray diffraction and X-ray reflectivity, as well as a Transmission Electron Microscopy cross section, taken as a physical reference. This study validates quantitatively the spectro-ellipsometry as a suitable routine tool to measure accurately both thickness and complex refractive index of the LSMO thin film, picturing their peculiar electrical behaviour between both metallic and insulating phases. The relative error on the thickness measurement between X-ray and ellipsometry is less than 5%. The LSMO complex refractive index enabled also a simultaneous estimation of further material properties, such as the optical gap ωg or the mass density ρm, determined with less than 1.5% relative error compared to X-ray reflectivity results.