Ethylene diamine tetra-acetic acid (EDTA) was used to prepare spinel LiMn 2 O 4 at 650 °C. The prepared sample by EDTA (E-LiMn 2 O 4 ) is compared with another spinel sample (C-LiMn 2 O 4 ) prepared by citric acid as a common chelating agent at the higher temperature (800 C) adjusted to obtain the same size and shape of the particles as in (E-LiMn 2 O 4 ) sample, as probed by SEM and TEM images. Investigation of both samples by X-ray diffraction showed that both samples have the single phase cubic spinel LiMn 2 O 4 phase with space group Fd-3m. Vibration properties obtained from Raman scattering (RS) and Fourier Transform Infra-Red (FTIR) spectroscopy for both samples are identical with spinel LiMn 2 O 4 structure. 7 Li MAS NMR and XPS spectra show that the amount of Mn 4+ is larger in LiMn 2 O 4 sample prepared by citric acid. LiMn 2 O 4 sample prepared using EDTA as chelating agent has better structural properties, but the improvement of the electrochemical properties is much smaller than the results reported in the literature for lamellar compounds and silicate materials. This is attributed to the features specific to the spinel, which limit both the capacity and cycle ability: dissolution of manganese and Jahn-Teller distortions associated to Mn 3+ ions, that are not modified by the choice of chelating agent.
This work aimed at synthesizing MoO3 and MoO2 by a facile and cost-effective method using extract of orange peel as a biological chelating and reducing agent for ammonium molybdate. Calcination of the precursor in air at 450 °C yielded the stochiometric MoO3 phase, while calcination in vacuum produced the reduced form MoO2 as evidenced by X-ray powder diffraction, Raman scattering spectroscopy, and X-ray photoelectron spectroscopy results. Scanning and transmission electron microscopy images showed different morphologies and sizes of MoOx particles. MoO3 formed platelet particles that were larger than those observed for MoO2. MoO3 showed stable thermal behavior until approximately 800 °C, whereas MoO2 showed weight gain at approximately 400 °C due to the fact of re-oxidation and oxygen uptake and, hence, conversion to stoichiometric MoO3. Electrochemically, traditional performance was observed for MoO3, which exhibited a high initial capacity with steady and continuous capacity fading upon cycling. On the contrary, MoO2 showed completely different electrochemical behavior with less initial capacity but an outstanding increase in capacity upon cycling, which reached 1600 mAh g−1 after 800 cycles. This outstanding electrochemical performance of MoO2 may be attributed to its higher surface area and better electrical conductivity as observed in surface area and impedance investigations.
Silver nanoparticles (AgNPs) and silver/quartz nanocomposite (Ag/Q)NPs)) were synthesized by sol-gel method using table sugar as chelating agent. The synthesized nanosized materials were used for mercury ions adsorption from aqueous solutions. The materials were characterized by X-ray diffraction (XRD), Transmission Electron microscope (TEM), and surface area (BET). Adsorption of Hg2+ (10 mg/l) is strongly dependent on time, initial metal concentration, dose of adsorbent and pH value. Silver/quartz nanocomposite ((Ag/Q)NPs)) shows better efficiency than individual silver nanoparticles (AgNPs). This composite removed mercury ions from the aqueous solution with efficiency of 96% at 60 min with 0.5g adsorbent dosage at pH 6. The adsorption process explained well by the pseudo-second-order kinetic model. In conclusion silver/quartz nanocomposite (Ag/Q)NPs)) shows higher removal efficiency for mercury ions from aqueous solutions than individual silver naoparticles (AgNPs) or quartz (Q).
An amorphous MomO3m−1/carbon nanocomposite (m ≈ 5) is fabricated from a citrate–gel precursor heated at moderate temperature (500 °C) in inert (argon) atmosphere. The as-prepared Mo5O14-type/C material is compared to α-MoO3 synthesized from the same precursor in air. The morphology and microstructure of the as-prepared samples are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman scattering (RS) spectroscopy. Thermal gravimetry and elemental analysis indicate the presence of 25.8 ± 0.2% of carbon in the composite. The SEM images show that Mo5O14 is immersed inside a honeycomb-like carbon matrix providing high surface area. The RS spectrum of Mo5O14/C demonstrates an oxygen deficiency in the molybdenum oxide and the presence of a partially graphitized carbon. Outstanding improvement in electrochemical performance is obtained for the Mo5O14 encapsulated by carbon in comparison with the carbon-free MoO3.
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