X-ray Photoelectron Spectroscopy Investigation Research Articles

XPS Investigation of Magnetization Reduction Behavior and Kinetics of Oolitic Hematite in Gas-Based Roasting

Magnetization reduction roasting is an important method for the utilization of oolitic magnetite. In this study, the magnetization reduction behavior and kinetics of oolitic hematite in gas-based roasting were systematically investigated by X-ray photoelectron spectroscopy (XPS). The results revealed that under optimal roasting conditions of 650 °C, a roasting time of 60 min, and a CO concentration of 30%, the magnetization reduction rate of the roasted product reached 44.34%. Furthermore, the weak magnetic separation concentrate presented a TFe of 58.09% and a concentrate iron recovery of 94.3%. The results of the XPS spectrum indicated that the peak area ratio (Fe2+/Fe3+) gradually increased with an increase in roasting temperature, roasting time, and CO concentration, while over-reduction occurred when the roasting temperature exceeded 750 °C. The investigation of magnetization roasting kinetics for varying particle sizes demonstrated that the magnetization reduction process is controlled by chemical reaction, with a corresponding activation energy range of 42.96 kJ/mol to 63.29 kJ/mol, indicating the particle size has little effect on the magnetization reduction of oolitic hematite.

A comparative analysis of corrosion assessment techniques for steel in reinforced concrete exposed to brine water environments

Abstract Corrosion assessment of steel-reinforced concrete specimens submerged in synthetic brine water with various chloride concentrations for 1–16 weeks was performed. Mass loss measurements combined with electrochemical techniques – half-cell potential, linear polarization (LP), and electrochemical impedance spectroscopy (EIS) – were employed. The results obtained from all corrosion assessments – on-site testing (half-cell potential measurements), laboratory scale (LP and EIS measurements), and destructive testing (mass loss or immersion measurements) – exhibited remarkable consistency, complementarity, and mutual supportiveness. Corrosion rate (CR) values from mass loss were close to those obtained from LP and EIS. The corrosion resistance decreased with increasing chloride concentration and immersion time, as indicated by the highest CR, Ca2+, and Fe2+ concentrations, and the lowest half-cell potential and polarization resistance. X-ray photoelectron spectroscopy investigation on the corroded steel surface revealed Fe(III) oxides and hydroxides and Fe(III) (FeCl3), corresponding to the reduction in polarization resistance in the LP and EIS results.

Enhanced Adsorption of Methyl Orange from Aqueous Phase Using Chitosan-Palmer Amaranth Biochar Composite Microspheres.

To develop valuable applications for the invasive weed Palmer amaranth, we utilized it as a novel biochar source and explored its potential for methyl orange adsorption through the synthesis of chitosan-encapsulated Palmer amaranth biochar composite microspheres. Firstly, the prepared microspheres were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy and were demonstrated to have a surface area of 19.6 m2/g, a total pore volume of 0.0664 cm3/g and an average pore diameter of 10.6 nm. Then, the influences of pH, dosage and salt type and concentration on the adsorption efficiency were systematically investigated alongside the adsorption kinetics, isotherms, and thermodynamics. The results reveal that the highest adsorption capacity of methyl orange was obtained at pH 4.0. The adsorption process was well fitted by a pseudo-second-order kinetic model and the Langmuir isotherm model, and was spontaneous and endothermic. Through the Langmuir model, the maximal adsorption capacities of methyl orange were calculated as 495.0, 537.1 and 554.3 mg/g at 25.0, 35.0 and 45.0 °C, respectively. Subsequently, the adsorption mechanisms were elucidated by Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy investigations. It is indicated that electrostatic interactions, hydrogen bonding, π-π interactions and hydrophobic interactions between methyl orange and the composite microspheres were pivotal for the adsorption process. Finally, the regeneration studies demonstrated that after five adsorption-desorption cycles, the microspheres still maintained 93.6% of their initial adsorption capacity for methyl orange. This work not only presents a promising method for mitigating methyl orange pollution but also offers a sustainable approach to managing Palmer amaranth invasion.

Interface defect formation for atomic layer deposition of SnO2 on metal halide perovskites

With the rapidly advancing perovskite solar cell (PSC) technology, dedicated interface engineering is critical for improving device stability. Atomic layer deposition (ALD) grown metal oxide films have drawn immense attention for the fabrication of stable PSC. Despite the advantages of ALD, the deposition of metal oxides directly on bare perovskite has so far not been achieved without damaging the perovskite layer underneath. In addition, the changes to the physicochemical and electronic properties at the perovskite interface upon exposure to the ALD precursors can alter the material and hence device functionality. Herein, we report on a synchrotron-based hard X-ray photoelectron spectroscopy (HAXPES) investigation of the interface between metal halide perovskite (MHP) absorber and ALD-SnO2 electron transport layer. We find clear evidence for the formation of new chemical species (nitrogen compound, lead dihalides) and an upward band bending in the MHP and downward band bending in the SnO2 towards the MHP/ALD-SnO2 interface. The upward bending at the interface forms an electron barrier layer of ∼400 meV, which is detrimental to the PSC performance. In addition, we assess the effectiveness of introducing a thin interlayer of the organic electron transport material Phenyl-C61-butyric acid methyl ester (PCBM) between MHP and ALD-SnO2 to mitigate the effects of ALD deposition.

Preparation and Characterization of Porous Carbon Material from Banana Pseudo-Stem

In this work, pseudo-stem of a banana plant was used as a sustainable and affordable source to prepare porous carbon materials (PCM) on a large scale. After fine treatment, the material was annealed at 500, 600, and 700 °C using a tube furnace under nitrogen flow. The prepared materials were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). FT-IR spectra show that the broad peak at the range of 1110-1160 cm-1 comes from the superimposed peaks of C-N for a single or more than one functional group which debunks the possibility of generating nitrogen-doped carbon. TEM and SEM analyses confirmed the porous structure of PCM with the pores connected to one, and a spongy structure was observed in the prepared carbon material. XRD analysis revealed that the carbon materials are crystalline. XPS investigation provided information regarding the dimension of which elements are present in the valence states and constituent elements, depicting the presence of a dominant graphitic C1speak at approximately 284 eV, along with a distinct O1s peak at around 532 eV. Additionally, a relatively weaker N1s peak (approximately 400 eV) was observed. Dhaka Univ. J. Sci. 72(1): 63-70, 2024 (January)

Structural Parameters and Behavior in Simulated Body Fluid of High Entropy Alloy Thin Films.

The structure, composition and corrosion properties of thin films synthesized using the Pulsed Laser Deposition (PLD) technique starting from a three high entropy alloy (HEA) AlCoCrFeNix produced by vacuum arc remelting (VAR) method were investigated. The depositions were performed at room temperature on Si and mirror-like polished Ti substrates either under residual vacuum (low 10-7 mbar, films denoted HEA2, HEA6, and HEA10, which were grown from targets with Ni concentration molar ratio, x, equal to 0.4, 1.2, and 2.0, respectively) or under N2 (10-4 mbar, films denoted HEN2, HEN6, and HEN10 for the same Ni concentration molar ratios). The deposited films' structures, investigated using Grazing Incidence X-ray Diffraction, showed the presence of face-centered cubic and body-centered cubic phases, while their surface morphology, investigated using scanning electron microscopy, exhibited a smooth surface with micrometer size droplets. The mass density and thickness were obtained from simulations of acquired X-ray reflectivity curves. The films' elemental composition, estimated using the energy dispersion X-ray spectroscopy, was quite close to that of the targets used. X-ray Photoelectron Spectroscopy investigation showed that films deposited under a N2 atmosphere contained several percentages of N atoms in metallic nitride compounds. The electrochemical behavior of films under simulated body fluid (SBF) conditions was investigated by Open Circuit Potential (OCP) and Electrochemical Impedance Spectroscopy measurements. The measured OCP values increased over time, implying that a passive layer was formed on the surface of the films. It was observed that all films started to passivate in SBF solution, with the HEN6 film exhibiting the highest increase. The highest repassivation potential was exhibited by the same film, implying that it had the highest stability range of all analyzed films. Impedance measurements indicated high corrosion resistance values for HEA2, HEA6, and HEN6 samples. Much lower resistances were found for HEN10 and HEN2. Overall, HEN6 films exhibited the best corrosion behavior among the investigated films. It was noticed that for 24 h of immersion in SBF solution, this film was also a physical barrier to the corrosion process, not only a chemical one.

Visible light-responsive Ce-doped ZnO ceramic nanostructures as effective photocatalysts for removal of persistent organic pollutants from contaminated waters

Cerium-doped zinc oxide (ZnO) ceramic nanostructures were conceived and prepared by means of electrospinning-calcination method. Morphological analysis based on scanning electron microscopy (SEM) disclosed a transition from spherical to rod-shaped features in ZnO ceramic nanostructures upon cerium (Ce) doping amount. Powder X-ray diffraction (XRD) indicated that the unit cell parameters remained unchanged for doped ZnO, while a new diffraction peak at 2θ = 28.57° occurred above 0.5% Ce, corresponding to cubic CeO2. The results are further supported by X-ray Photoelectron Spectroscopy (XPS) investigations, which clearly confirmed the occurrence of Ce4+ ions upon the increase of Ce incorporation during the synthesis. Photocatalytic screening assays for methylene blue (MB) degradation using a visible light source, demonstrated superior performance for the doped material with 0.1% Ce content, yielding the highest pseudo-first-order rate constant (k = 4.795 × 10−2 min−1). Additionally, the best catalyst ZnO:Ce (0.1%), showed rate constants of 1.018 × 10−2 min−1 and 3.675 × 10−2 min−1 for photodegradation of metronidazole (MNZ) and ciprofloxacin (CIP), respectively, under the established optimal conditions. The catalyst stability was confirmed through multiple reuse cycles. The present study points out the effective Ce-doped ZnO nanostructures for versatile photocatalytic applications.

Thermally exfoliated graphene oxide doped microporous bio-nanocomposite hydrogel: A promising substrate for biomedical application

Hydrogels have demonstrated significant promise as flexible/wearable sensors for the diagnosis, monitoring, and delivery of personalized medicine for health issues and deficiencies. To this end, a novel approach was employed towards the development of a hybrid hydrogel nanocomposite-based biosensing substrate. The hierarchical hydrogel matrix derived by using polyaniline (PANI)/polyvinyl-alcohol (PVA) biopolymer-matrix, was reinforced with in-house synthesized thermally exfoliated graphene-oxide (TEGO). Fourier transform infrared spectroscopy (FT-IR) confirmed the interfacial-interactions between hydroxyl groups and functional groups of TEGO, a conducive property for immobilization and catalytic activities. X-ray photoelectron spectroscopy (XPS) investigation of the developed nanocomposite hydrogel demonstrated that the addition of nanofiller facilitated the ordered structure of nanocomposite hydrogel. Further, field emission scanning electron microscopy (FE-SEM) investigations revealed interconnected porous microstructure of the nanocomposites, assisted by nucleating effect of TEGO, a supporting micro-environment for the transportation of biomolecules. Impedance analysis and hall effect studies showed that the nanocomposite hydrogel substrate was highly conductive. In vitro cytocompatibility results demonstrated excellent biocompatibility of the bio-nanocomposite hydrogels. Cyclic-voltammetry analysis indicated a reduction in current on the surface due to long-range shattered conjugated network of TEGO and PANI in presence of functional groups. Overall, this study indicates that developed bio-nanocomposite hydrogel substrates are promising candidates for biomedical applications.

Nickel-doped vanadium pentoxide (Ni@V2O5) nanocomposite induces apoptosis targeting PI3K/AKT/mTOR signaling pathway in skin cancer: An in vitro and in vivo study

In the present study, the vanadium pentoxide (V2O5) nickel-doped vanadium pentoxide (Ni@V2O5) was prepared and determined for in vitro anticancer activity. The structural characterization of the prepared V2O5 and Ni@V2O5 was determined using diverse morphological and spectroscopic analyses. The DRS-UV analysis displayed the absorbance at 215 nm for V2O5 and 331 nm for Ni@V2O5 as the primary validation of the synthesis of V2O5 and Ni@V2O5. The EDS spectra exhibited the presence of 30% of O, 69% of V, and 1% of Ni and the EDS mapping showed the constant dispersion. The FE-SEM and FE-TEM analysis showed the V2O5 nanoparticles are rectangle-shaped and nanocomposites have excellent interfaces between nickel and V2O5. The X-ray photoelectron spectroscopy (XPS) investigation of Ni@V2O5 nanocomposite endorses the occurrence of elements V, O, and Ni. The in vitro MTT assay clearly showed that the V2O5 and Ni@V2O5 have significantly inhibited the proliferation of B16F10 skin cancer cells. In addition, the nanocomposite produces the endogenous reactive oxygen species in the mitochondria, causes the mitochondrial membrane and nuclear damage, and consequently induces apoptosis by caspase 9/3 enzymatic activity in skin cancer cells. Also, the western blot analysis showed that the nanocomposite suppresses the oncogenic marker proteins such as PI3K, Akt, and mTOR in the skin cancer cells. Together, the results showed that Ni@V2O5 can be used as an auspicious anticancer agent against skin cancer.

Enhancing La(III) biosorption and biomineralization with Micromonospora saelicesensis: Involvement of phosphorus and formation of monazite nano-minerals

The release of rare earth elements (REEs) from mining wastes and their applications has significant environmental implications, necessitating the development of effective prevention and reclamation strategies. The mobility of REEs in groundwater due to microorganisms has garnered considerable attention. In this study, a La(III) resistant actinobacterium, Micromonospora saelicesensis KLBMP 9669, was isolated from REE enrichment soil in GuiZhou, China, and evaluated for its ability to adsorb and biomineralize La(III). The findings demonstrated that M. saelicesensis KLBMP 9669 immobilized La(III) through the physical and chemical interactions, with immobilization being influenced by the initial La(III) concentration, biomass, and pH. The adsorption kinetics followed a pseudo-second-order rate model, and the adsorption isotherm conformed to the Langmuir model. La(III) adsorption capacity of this strain was 90 mg/g, and removal rate was 94 %. Scanning electron microscope (SEM) coupled with energy dispersive X-ray spectrometer (EDS) analysis revealed the coexistence of La(III) with C, N, O, and P. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) investigations further indicated that carboxyl, amino, carbonyl, and phosphate groups on the mycelial surface may participate in lanthanum adsorption. Transmission electron microscopy (TEM) revealed that La(III) accumulation throughout the M. saelicesensis KLBMP 9669, with some granular deposits on the mycelial surface. Selected area electron diffraction (SAED) confirmed the presence of LaPO4 crystals on the M. saelicesensis KLBMP 9669 biomass after a prolonged period of La(III) accumulation. This post-sorption nano-crystallization on the M. saelicesensis KLBMP 9669 mycelial surface is expected to play a crucial role in limiting the bioimmobilization of REEs in geological repositories.

Anisotropic etching mechanisms of 4H-SiC: Experimental and first-principles insights

Molten-alkali etching has been widely used to reveal dislocations in 4H silicon carbide (4H-SiC), which has promoted the identification and statistics of dislocation density in 4H-SiC single crystals. However, the etching mechanism of 4H-SiC is limited misunderstood. In this letter, we reveal the anisotropic etching mechanism of the Si face and C face of 4H-SiC by combining molten-KOH etching, X-ray photoelectron spectroscopy (XPS) and first-principles investigations. The activation energies for the molten-KOH etching of the C face and Si face of 4H-SiC are calculated to be 25.09 and 35.75 kcal/mol, respectively. The molten-KOH etching rate of the C face is higher than the Si face. Combining XPS analysis and first-principles calculations, we find that the molten-KOH etching of 4H-SiC is proceeded by the cycling of the oxidation of 4H-SiC by the dissolved oxygen and the removal of oxides by molten KOH. The faster etching rate of the C face is caused by the fact that the oxides on the C face are unstable, and easier to be removed with molten alkali, rather than the C face being easier to be oxidized.

Indium-Based Silica Materials: Sustainable Syntheses Combined with a Challenging Insertion in SiO2 Mesoporous Structures.

Optimized sustainable procedures in both acidic and basic conditions are considered to meet some of the current environmental challenges of the scientific community. In this paper, the successful syntheses of two classes of indium-based silica nanomaterials are reported. Both procedures were conceived to enhance the sustainability of the synthesis methods and promote their preparations at room temperature while avoiding the hydrothermal treatment under static conditions at 100 °C. A fast, room-temperature synthesis of porous nanospheres was conceived together with an "acid-free" procedure for SBA-15-like materials. Moreover, the isomorphic substitution of silicon with indium was achieved. All the materials were deeply characterized to probe their structural, textural and morphological properties (e.g., transmission electron microscopy, N2 physisorption, ss MAS NMR of 29Si). The high specific surface area and the mesoporosity were always preserved even under the mild reaction conditions employed. The honeycomb structure and the spherical morphology of SBA-15-like materials and nanospheres, respectively, were also observed. The insertion of indium was confirmed via X-ray photoelectron spectroscopy (XPS) investigations.

High-Sensitivity H2 and CH4 SAW Sensors with Carbon Nanowalls and Improvement in Their Performance after Plasma Treatment

We have developed surface acoustic wave (SAW) sensors with high sensitivity and a reversible response at room temperature (RT). The sensitive area of the sensor was prepared from vertically aligned graphene sheets, like carbon nanowalls (CNWs), which were deposited onto the quartz SAW sensor substrate. The CNWs were obtained by RF plasma-enhanced chemical vapor deposition (PECVD) at 600 °C, and their sensitivity was subsequently enhanced through hydrogen plasma treatment. The SAW sensors were tested at H2 and CH4 at RT, and they exhibited a reversible response for both gases at concentrations between 0.02% and 0.1%, with a detection limit of a few ppm. The additional hydrogen plasma treatment preserved the lamellar structure, with slight modifications to the morphology of CNW edges, as observed by scanning electron microscopy (SEM). X-ray photoelectron spectroscopy (XPS) investigations revealed the presence of new functional groups, a significant number of defects and electron transitions after the treatment. Changes in the chemical state on the CNW surface are most probably responsible for the improved gas adsorption after plasma treatment. These results identify CNWs as a promising material for designing new SAW sensors, with the possibility of using plasma treatments to enhance the detection limit below the ppm level.

Germanium surface cleaning and ALD of a protective boron nitride overlayer

Germanium exhibits superior hole and electron mobility compared with silicon, making it a promising candidate for replacement of silicon in certain future CMOS applications. In such applications, achieving atomically clean Ge surfaces and the subsequent deposition of ultrathin passivation barriers without interfacial reaction are critical. In this study, we present in situ x-ray photoelectron spectroscopy (XPS) investigations of hydrocarbon removal from the Ge surface utilizing atomic oxygen at room temperature, as well as removal of hydrocarbons and of germanium oxide (GeO2) through atomic hydrogen treatment at 350 °C. Subsequently, atomic layer deposition (ALD) was used to create a protective layer of hexagonal boron nitride (h-BN) with an average thickness of 3 monolayers (ML). Tris(dimethylamino)borane and ammonia precursors were utilized at 450 °C for the deposition process. Intermittent in situ XPS analysis during ALD confirmed h-BN growth, stoichiometry, and the absence of interfacial reaction with Ge. XPS analysis after subsequent exposure of the Ge film with a h-BN overlayer of ∼9 Å average thickness to 7.2 × 104 l of atomic O (O3P) at room temperature yielded no evidence of Ge oxidation, with only the surface layer of the h-BN film exhibiting oxidation. These results present a practical and scalable route toward the preparation of clean Ge surfaces and subsequent deposition of protective, nanothin h-BN barriers for subsequent processing.

Insights into the properties and possible bonding states of radiofrequency-magnetron-sputtered indium tin oxide thin films acquired using ultraviolet–visible spectroscopy data for cost-effective material characterization

Indium tin oxide (Sn-doped In2O3) is an optical material that is widely utilized in designing modern optoelectronic devices. To demonstrate the efficiency of ultraviolet–visible spectroscopy as a primary analysis tool for thin-film characterization, Sn-doped In2O3 films were deposited under untreated and annealed conditions. The optical parameters of these films were determined based on the transmission–reflection spectra recorded by an ultraviolet–visible spectroscopy laboratory setup. Through four-point probing, energy dispersive spectroscopy, and contact angle measurements, the electronic-band structures and chemical bonding states of the thin films were estimated. The transmission spectra confirmed that the post-annealing treatment promoted film homogeneity. Deeper insights into the optical parameters revealed that annealing encouraged Sn atom incorporation into the film structure and better stable phase formation. The incorporation of Sn atoms resulted in the substitution of Sn4+ into the In3+ sites of the In2O3 lattice and formation of the SnO phase. Notably, our evaluation of the film properties based on data acquired from ultraviolet–visible spectroscopy revealed good consistency with the data acquired from Hall-effect, X-ray diffractometry, and X-ray photoelectron spectroscopy investigations.

Plasma power effect on crystallinity and density of AlN films deposited by plasma enhanced atomic layer deposition

Aluminum nitride (AlN) film is a promising material which is used in various fields. In this study, AlN films with different plasma powers were grown by remote plasma atomic layer deposition. Saturation experiments have been applied in the plasma power between 1000 and 3000 W. The influence of plasma power on preferential orientation, chemical, optical, and electrical properties of AlN films are investigated. AlN films displayed multiphase hexagonal wurtzite crystal structure with (002) preferential orientation for higher plasma power, while the predominant orientation shifted toward (100) at lower plasma power. The optical emission spectroscopy analyses show that NH and NH2 radicals conduce to the deposition of AlN films and H radicals selectively dissociate Al–OH bonds which were on AlN film surface and etch deposition films. Atomic force microscopy measurements show that the 1500 W prepared AlN film with smallest surface roughness may be related to the relatively smaller concomitant crystal grains of (100) and (002). X-ray photoelectron spectroscopy investigation presents that oxygen content decreases as the plasma power increases. The obtained maximum value of dielectric constant and breakdown electrical field of AlN film deposited at 3000 W is 8.23 and 5.42 MV/cm, respectively.

Optoelectronic properties and optical transitions in low concentrated aluminum-doped tin oxide thin films

The structural, chemical, surface morphology, and optoelectronic characteristics of Al-doped SnO2 (ATO) films are investigated and a comprehensive analysis of the obtained results is presented. All films are shown to have a polycrystalline tetragonal rutile structure by X-ray diffraction (XRD) measurements, and the single-phase nature of the structure is proved by detailed X-ray photoelectron spectroscopy (XPS) investigations. Two mechanisms of Al incorporation into the SnO2 lattice were evident by XRD and XPS measurements. Comprehensive XPS, XRD, and Hall effect investigations showed a clear relation between the charge carrier concentration, crystallite size, and the concentration of oxygen vacancy defects. Through a comprehensive analysis of the photoluminescence (PL) measurements, we determined the positions of various defect states within the bandgap. Using a thorough analysis of the optical absorption measurements, we have successfully demonstrated the presence of four direct optical transitions with energies ranging from 3.84 to 5.10 eV, and by considering the Moss–Burstein effect and the Urbach tailing phenomenon, it was shown that the first transition energy (E1) corresponds to the direct optical transition across the Γ3+−Γ1+ forbidden energy gap. The other three transitions are ascribed to electronic transitions from the valence band states Γ5− and Γ5+ to different defect states within the bandgap.

Multilayer Epitaxial Heterostructures with Multi-Component III-V:Fe Magnetic Semiconductors.

Three-layer structures based on various multi-component films of III-V semiconductors heavily doped with Fe were grown using the pulsed laser sputtering of InSb, GaSb, InAs, GaAs and Fe solid targets. The structures comprising these InAsSb:Fe, InGaSb:Fe and InSb:Fe layers with Fe concentrations up to 24 at. % and separated by GaAs spacers were deposited on (001) i-GaAs substrates at 200 °C. Transmission electron microscopy showed that the structures have a rather high crystalline quality and do not contain secondary-phase inclusions. X-ray photoelectron spectroscopy investigations revealed a significant diffusion of Ga atoms from the GaAs regions into the InAsSb:Fe layers, which has led to the formation of an InGaAsSb:Fe compound with a Ga content up to 20 at. %. It has been found that the ferromagnetic properties of the InAsSb:Fe magnetic semiconductor improve with an increasing Sb:As ratio. It has been concluded that the indirect ferromagnetic exchange interaction between Fe atoms occurs predominantly via Sb atoms.

Mass spectrometry and in situ x-ray photoelectron spectroscopy investigations of organometallic species induced by the etching of germanium, antimony and selenium in a methane-based plasma

Organometallic positive ions were identified in inductively coupled plasmas by means of mass spectrometry during the etching of Ge, Sb, Se materials. A preliminary study was focused on identifying M x H y + (M = Ge, Sb, Se) positive ion clusters during a H2/Ar etching process. The methane addition to the H2/Ar mixture generates CH x reactive neutral species. The latter react with the metalloids within gas phase to form M x C y H z + organometallic ions. In addition, the etching of Sb2Se3 and Ge19.5Sb17.8Se62.7 bulk targets forms mixed products via ion-molecule reactions as evidenced by the presence of SeSbC x H y + ion clusters. Changes in surface composition induced by the newly formed organometallic structures were investigated using in situ x-ray photoelectron spectroscopy. In the case of the Ge and Sb surfaces, (M)–M–C x environments broadened the Ge 2p3/2, Ge 3d, Sb 3d and Sb 4d spectra to higher values of binding energy. For the Se surface, only the hydrogen and methyl bonding could explain the important broadening of the Se 3d core level. It was found that the Ge39Se61 thin film presents an induced (Ge)–Ge–Se entity on the Ge 2p3/2 and Ge 3d core levels.

Sm doped ZnO-SnO2 nanocomposites with improved photo-degradation strength and antibacterial properties

In this work, we devoted our effort to synthesize rare-earth (Sm3+) doped ZnO-SnO2 nanocomposites by sol-gel method to address issues like wastewater treatment and minimization of bacterial infection. Successful formation of multi-phase nanocomposites of hexagonal ZnO and tetragonal SnO2 has been confirmed by x-ray diffraction (XRD) analysis. The effect of Sm doping is understood from the enhancement in ZnO grain growth and shift in diffraction peaks. The morphology study by FESEM reveals the variation in sample morphology with Sm doping with energy-dispersive analysis of x-ray (EDAX) study providing the confirmation on the existence of Sm ions in the crystal lattice of ZnO-SnO2 heterostructure. Transmission electron microscopic (TEM) study manifests the formation of two distinct types of particles (hexagonal & spherical) corresponding to ZnO and SnO2 which has been further clarified from the measurement of lattice spacing from the high-resolution TEM images and indexing of selected area electron diffraction (SAED) pattern. The near band edge emission (NBE) of ZnO is blue shifted along with the evolution of oxygen vacancy defects which induced new bands at 488 nm and 613 nm upon Sm doping. Further, intra-4f transitions of Sm3+ ions have also been observed at 560 nm, 590 nm and 638 nm linked to 4G5/2– 6HJ (J = 5/2, 7/2, 9/2) transitions. The Zn, Sn, O, and Sm elements are confirmed to exist in the nanocomposite according to the X-ray photoelectron spectroscopy (XPS) investigation which provided information on the chemical composition and electronic states of the material. Photocatalytic degradation study of toxic environmental dyes like methylene blue (MB), Congo red (CR) and methyl orange (MO) shows that Sm3+ ions in ZnO/SnO2 helps to enhance the degradation efficiency by the formation of Z-scheme heterojunctions between ZnO and SnO2. This allows the delay in recombination rate of the photoinduced electron/hole pairs. The antibacterial behavior of the prepared nanocomposites against E. Coli and S. Aureus has also been studied in detail which demonstrates improved antibacterial efficiency of the samples.