scholarly journals Testing the Efficacy of the Synthesis of Iron Antimony Sulfide Powders from Single Source Precursors

Inorganics ◽  
2021 ◽  
Vol 9 (8) ◽  
pp. 61
Author(s):  
Fadiyah Makin ◽  
Dalal Alzahrani ◽  
Firoz Alam ◽  
Floriana Tuna ◽  
David J. Lewis

The antimony-iron sulfide system in general does not produce alloys below 540 °C from traditional solid-state methods. However, single source precursors have been known to produce unexpected products that arise from kinetically trapped polymorphs. In this paper, we test the efficacy of this approach toward the Fe-Sb-S system. Antimony and iron diethyldithiocarbamate complexes of the form Sb[S2CN(Et2)]3 (1) and Fe[S2CN(Et2)]3 (2) were synthesised, characterised, and used as single-source precursors for the preparation of Sb2S3, FexSy, and mixed iron antimony sulfide Sb2(1−x)Fe2xS3 (0 ≥ x ≥ 1) powders using the solvent-less thermolysis method at different temperatures ranging from 300 to 475 °C. The effect of different mole fractions of the iron precursor was evaluated on morphology, shape, and optical and magnetic properties of Sb2(1−x)Fe2xS3 (0 ≥ x ≥ 1). The obtained powders were characterized by X-ray diffraction (XRD), Raman spectroscopy scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, magnetometer measurement, and UV/vis/NIR spectroscopy. The results demonstrated that the crystalline structure, morphology, and elemental composition of the samples changed with the mole fraction of the precursor. There was significant phase separation between Sb and Fe sulfides noted from EDX spectroscopic mapping, yet an optoelectronic study monitoring the direct band gap energy of antimony sulfide shows that the band gap energy increases as a function of Fe content, which suggests limited alloying is possible from the single source route.

2017 ◽  
Vol 889 ◽  
pp. 234-238
Author(s):  
Mohd Hasmizam Razali ◽  
Nur Arifah Ismail ◽  
Mahani Yusoff

Pure and F doped TiO2 nanotubes was synthesized using simple hydrothermal method. The hydrothermal was conducted using teflon-liner autoclave and maintained at 150oC for 24 hours. The characterization of synthesised product was carried out using x-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive of x-ray spectroscopy (EDX) and ultra violet – visible light diffuse reflectance spectroscopy (UV-Vis DRS) for band gap measurements. XRD patterns indicated that anatase TiO2 phase was remained after F doping suggested that fluorine was highly dispersed into TiO2 by substituted with O in the TiO2 lattice to formed TiO2-xFx solid solution. Morphology investigation using TEM found out small diameter of nanotubes structure within 8 – 10 nm of pure and F doped TiO2 nanotubes. The band gap energy (Eg) of both nanotubes samples were almost similar proposing that F doping does not modify the band gap energy.


Crystals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 968
Author(s):  
Reina Galeazzi Isasmendi ◽  
Isidro Juvenal Gonzalez Panzo ◽  
Crisóforo Morales-Ruiz ◽  
Román Romano Trujillo ◽  
Enrique Rosendo ◽  
...  

Copper oxide (CuO) films were deposited onto glass substrates by the microwave assisted chemical bath deposition method, and varying the pH of the solution. The pH range was varied from 11.0 to 13.5, and the effects on the film properties were studied. An analytical study of the precursor solution was proposed to describe and understand the chemical reaction mechanisms that take place in the chemical bath at certain pH to produce the CuO film. A series of experiments were performed by varying the parameters of the analytical model from which the CuO films were obtained. The crystalline structure of the CuO films was studied using X-ray diffraction, while the surface morphology, chemical composition, and optical band-gap energy were analyzed by scanning electron microscopy, X-ray photoelectron spectroscopy, and UV–Vis spectrophotometry, respectively. The CuO films obtained exhibited a monoclinic crystalline phase, nanostructured surface morphology, stoichiometric Cu/O ratio of 50/50 at%, and band-gap energy value of 1.2 eV.


Author(s):  
Anuar Kassim ◽  
Tan Wee Tee ◽  
Ho Soon Min ◽  
Shanthi Monohorn ◽  
Saravanan Nagalingam

PbSe thin films are prepared by chemical bath deposition technique over microscope glass substrates from an aqueous acidic bath containing lead nitrate and sodium selenate. The influence of bath temperature on the properties of PbSe film is investigated. The X-ray diffraction analysis showed the deposited films were polycrystalline and having the (111) orientation. The surface morphology study revealed that the grains have cubic shape crystal. The band gap energy was decreased from 2.0 to 1.3 eV as the bath temperature was increased from 40 to 80°C. The films deposited at 80°C showed good crystallinity and uniformly distributed over the surface of substrate with larger grain sizes. Therefore, the optimum bath temperature is 80°C. Keywords: Lead selenide; X-ray diffraction; Band gap energy; Chemical bath deposition; Thin films DOI: 10.3126/kuset.v6i2.4021Kathmandu University Journal of Science, Engineering and Technology Vol.6. No II, November, 2010, pp.126-132


Nanomaterials ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 3427
Author(s):  
Is Fatimah ◽  
Gani Purwiandono ◽  
Putwi Widya Citradewi ◽  
Suresh Sagadevan ◽  
Won-Chun Oh ◽  
...  

In this work, photoactive nanocomposites of ZnO/SiO2 porous heterostructures (PCHs) were prepared from montmorillonite clay. The effects of preparation methods and Zn content on the physicochemical features and photocatalytic properties were investigated. Briefly, a comparison of the use of hydrothermal and microwave-assisted methods was done. The Zn content was varied between 5 and 15 wt% and the characteristics of the nanomaterials were also examined. The physical and chemical properties of the materials were characterized using X-ray diffraction, diffuse-reflectance UV-Vis, X-ray photoelectron spectroscopy, and gas sorption analyses. The morphology of the synthesized materials was characterized through scanning electron microscopy and transmission electron microscopy. The photocatalytic performance of the prepared materials was quantified through the photocatalytic degradation of methyl violet (MV) under irradiation with UV and visible light. It was found that PCHs exhibit greatly improved physicochemical characteristics as photocatalysts, resulting in boosting photocatalytic activity for the degradation of MV. It was found that varied synthesis methods and Zn content strongly affected the specific surface area, pore distribution, and band gap energy of PCHs. In addition, the band gap energy was found to govern the photoactivity. Additionally, the surface parameters of the PCHs were found to contribute to the degradation mechanism. It was found that the prepared PCHs demonstrated excellent photocatalytic activity and reusability, as seen in the high degradation efficiency attained at high concentrations. No significant changes in activity were seen until five cycles of photodegradation were done.


Crystals ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 589 ◽  
Author(s):  
Lin ◽  
Guo ◽  
Dai ◽  
Lin ◽  
Hsu

In this work, we used the chemical vapor transport (CVT) method to grow PbI2 crystals using iodine as a self-transporting agent. The crystals’ structure, composition, and uniformity were confirmed by X-ray diffraction (XRD) and electron probe microanalysis (EPMA) measurements. We investigated the band gap energy using absorption spectroscopy measurements. Furthermore, we explored the temperature dependence of the band gap energy, which shifts from 2.346 eV at 300 K to 2.487 eV at 20 K, and extracted the temperature coefficients. A prototype photodetector with a lateral metal–semiconductor–metal (MSM) configuration was fabricated to evaluate its photoelectric properties using a photoconductivity spectrum (PC) and persistent photoconductivity (PPC) experiments. The resonance-like PC peak indicates the excitonic transition in absorption. The photoresponse ILight/IDark-1 is up to 200%.


2013 ◽  
Vol 772 ◽  
pp. 365-370 ◽  
Author(s):  
Mohd Hasmizam Razali ◽  
M.N. Ahmad-Fauzi ◽  
Abdul Rahman Mohamed ◽  
Srimala Sreekantan

Titanium dioxide (TiO2) nanoparticles were successfully synthesised by hydrothermal method using TiO2 microparticle powder (Merck) as precursor. TiO2 microparticles powder (~160 nm) was mixed with 10 M NaOH and treated hydrothermally at 150 °C and 2 MPa pressure in autoclave for 24 hours. After hydrothermal reaction was completed, the sample was washed, dried and heated at 500 °C for 2 hours to produce TiO2 nanoparticles. The synthesised nanoparticles were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and raman spectroscopy. UV-Vis DRS was used to determine the band gap energy. Field emissions and transmissions electron microscopy images revealed that nanoparticles obtained was about 14 nm. X-ray diffraction patterns showed that TiO2 nanoparticles were anatase phase (tetragonal). The band gap energy of TiO2 nanoparticles was determined to be 3.32 eV.


1996 ◽  
Vol 60 (402) ◽  
pp. 759-766 ◽  
Author(s):  
Laurent Van Haverbeke ◽  
Renaud Vochten ◽  
Karel Van Springel

AbstractChernikovite and meta-ankoleite were synthesized with a relatively high crystallinity and the compounds were identified by means of chemical analysis and X-ray diffraction. The infrared spectra were recorded and the bands assigned. From the luminescence spectra, the band-gap energy for both compounds was calculated as 2.35 eV, indicating that they must be considered as insulators. The dependence of the solubilities of these compounds on the acidity of the solution was studied, and the dominant ionic species were determined. The pKsp values of chernikovite and meta-ankoleite were found to be 22.73±0.24 and 24.30±0.81 respectively.


2019 ◽  
Vol 19 (11) ◽  
pp. 7139-7148 ◽  
Author(s):  
Suresh Sagadevan ◽  
Zaira Zaman Chowdhury ◽  
Mohd. Rafie Bin Johan ◽  
Fauziah Abdul Aziz ◽  
L. Selva Roselin ◽  
...  

In this work, a simple, co-precipitation technique was used to prepare un-doped, pure tin oxide (SnO2). As synthesized SnO2 nanoparticles were doped with Cu2+ ions. Detailed characterization was carried out to observe the crystalline phase, morphological features and chemical constituents with opto-electrical and magnetic properties of the synthesized nanoparticles (NPs). X-ray diffraction analysis showed the existence of crystalline, tetragonal structure of SnO2. Both the sample synthesized here showed different crystalline morphology. The band gap energy (Eg) of the synthesized sample was estimated and it was found to decrease from 3.60 to 3.26 eV. The band gap energy reduced due to increase in Cu2+ dopant amount inside the SnO2 lattice. Optical properties were analyzed using absorption spectra and Photoluminescence (PL) spectra. It was observed that Cu2+ ions incorporated SnO2 NPs exhibited more degradation efficiencies for Rhodamine B (RhB) dye compared to un-doped sample under UV-Visible irradiation. The dielectric characteristics of un-doped, pure and Cu2+ incorporated SnO2 nanoparticles were studied at different frequency region under different temperatures. The ac conductivity and impedance analysis of pure and Cu2+ incorporated SnO2 nanoparticles was also studied. The magnetic properties of the synthesized samples were analysed. Both the sample showed ferromagnetic properties. The research indicated that the Cu2+ ions doping can make the sample a promising candidate for using in the field of optoelectronics, magneto electronics, and microwave devices.


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