X-ray Diffractometer Patterns Research Articles

Permeability of Sand-Based Cemented Backfill under Different Stress Conditions: Effects of Confining and Axial Pressures

Sand-based cemented backfill (SBCB) mining technology is instrumental in utilizing coal resources buried under the water bodies. SBCB is exposed to the long-term action of mining-induced stresses in the goaf and groundwater permeating via microcracks along the rock strata. Studying the permeability evolution of SBCB under varying stress states is crucial for protecting coal and water resources below the aquifer. This study is focused on the influence law of different stress states on the SBCB permeability exposed to groundwater, which was tested under different axial and confining pressures using a laboratory seepage meter, particle size analyzer, scanning electron microscope (SEM), and X-ray diffractometer (XRD). Best-fitting quadratic polynomials linking the SBCB permeability with confining and axial pressures, respectively, were obtained via statistical processing of test results. The permeability gradually dropped within the elastic range as the confining and axial pressures increased. Moreover, an increase in the confining pressure caused a more dramatic reduction in the SBCB permeability than the axial pressure. Finally, the SBCB seepage mechanism under different stress states was revealed based on the particle size analysis, XRD patterns, and SEM microstructure. These findings are considered instrumental in substantiating safe mining of coal resources below the water bodies and above the confined groundwater.

Preparation of neodymium‐doped LiMnPO 4 /C cathode by sol‐gel method with excellent electrochemical performance for lithium‐ion batteries

The porous spherical structure neodymium-doped LiMn1−xNdxPO4/C nanoparticles have been prepared through glycolic acid-assisted sol-gel method. The neodymium-ion doping effect on the crystalline microstructure, crystal appearance, and electrochemical parameters of LiMnPO4/C cathodes have been detected by X-ray diffractometer (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), charge and discharge test, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) method. XRD patterns show that a proper amount of neodymium-ion doping could not change the host crystal structure; combined with EDS spectra, we could conclude that Nd3+ has successful embedding into the lattice structure of LiMnPO4/C. SEM analysis shows that the LiMn0.94Nd0.06PO4/C sample has the uniform and fine particles diameter distribution in comparison with other doped samples. The electrochemical measurement results indicate that the LiMn0.94Nd0.06PO4/C has the initial discharge specific capacity of 155.2 mAh/g at 0.05 C discharge rate; after 200 cycles, the capacity value reduces slightly to 138.7 mAh/g, the capacity retention rate is maintained at 89.4%. The LiMn0.94Nd0.06PO4/C has high-rate discharge performance with the specific capacity value of 128.0 mAh/g (10 C). The results conclude that a proper amount of neodymium-ion doping ratio could effectively enhance the lithium-ion diffusivity and improve high-rate performance of LiMnPO4 cathode materials.

Synthesis, structural elucidation, molecular modeling and antimicrobial studies of 6‐(2‐hydroxyphenylimine)‐2‐thioxotetrahydropyrimidin‐4(1H)‐one (L) Schiff base metal complexes

Solid complexes of Schiff base (L) with Co (II), Ni (II), Zn (II), Zr (IV) and Hg (II) in acetone as a solvent were synthesised and characterised by elemental analysis, magnetic measurements, melting point, molar conductivity, FT‐IR, UV–Vis., 1HNMR, X‐ray diffractometer (XRD) and thermogravimetric analyses (TG and DTG). Elemental analysis is in satisfactory correlation with the proposed chemical formulae of the complexes. The estimated molar conductivity of the compounds in 1 × 10−3 M DMF solution indicates the electrolytic existence of the examinated complexes and reported as 1:2 electrolytes for Co (II), Ni (II), Zr (IV) and Hg (II) complexes and 1:1 electrolytes for Zn (II) complex. Spectral and analytical results indicate that L chelated with metal ions as bidenate through the oxygen atom of the carbonyl group and nitrogen atom of azomethine group for all complexes. The XRD patterns demonstrate the non‐crystalline nature (amorphous) of the compounds (1), (4) and (5), but the compounds L, (2) and (3) lie between the amorphous and the crystalline characters. TG/DTG showed the compounds are thermally stable at room temperature and decomposed by raising the temperature to 600°C. The kinetic and thermodynamic parameters such as E*, ΔH*, ΔS* and ΔG* were calculated by using coats‐Redfern and Horowitz‐Metzger methods at n = 1 and n ≠ 1. Calculated values indicate more orderly activated complex formation. The measurements of the molecular modeling using density functional theory (DFT) confirm the structural geometry of the complexes, and the data showed the complexes are soft with respect to L where η varied from 0.068 to 0.077 eV and σ ranges from 12.987 to 14.706 eV, while η and σ for L are 0.109 and 9.174 eV−1, respectively. Complexes were tested for their in vitro antimicrobial activity against certain gram negative and gram positive bacteria in addition to two fungi species. The findings showed a clear increase in the anti‐tuberculosis activity due to complexion.

Preparation of Nanoparticle Porous-Structured BiVO4 Photoanodes by a New Two-Step Electrochemical Deposition Method for Water Splitting

In the synthesis method of a BiVO4 photoanode via BiOI flakes, a BiOI film is formed by electrochemical deposition in Step 1, and a vanadium (V) source solution is placed by drop-casting on the BiOI film in Step 2. Following this, BiVO4 particles are converted from the BiOI–(V species) precursors by annealing. However, it is challenging to evenly distribute vanadium species among the BiOI flakes. As a result, the conversion reaction to form BiVO4 does not proceed simultaneously and uniformly. To address this limitation, in Step 2, we developed a new electrochemical deposition method that allowed the even distribution of V2O5 among Bi–O–I flakes to enhance the conversion reaction uniformly. Furthermore, when lactic acid was added to the electrodeposition bath solution, BiVO4 crystals with an increased (040) peak intensity of the X-ray diffractometer (XRD) pattern were obtained. The photocurrent of the BiVO4 photoanode was 2.2 mA/cm2 at 1.23 V vs. reversible hydrogen electrode (RHE) under solar simulated light of 100 mW/cm2 illumination. The Faradaic efficiency of oxygen evolution was close to 100%. In addition, overall water splitting was performed using a Ru/SrTiO3:Rh–BiVO4 photocatalyst sheet prepared by the BiVO4 synthesis method. The corresponding hydrogen and oxygen were produced in a 2:1 stoichiometric ratio under visible light irradiation.

Ash analyses of bio-coal briquettes produced using blended binder

The behaviour of ash of fuel affects its thermal efficiency when in use. The ash analyses of bio-coal briquettes developed from lean grade coal and torrefied woody biomass have received limited intensive study. Therefore, the present study aims at analysing the ashes of briquette made from lean grade coal and torrefied woody biomass using blended coal tar pitch and molasses as the binder. Bio-coal briquettes were produced from coal and torrefied biomass in various hybrid ratios. Ashing of various briquettes was done in a muffle furnace at 850 °C for 3 h. Mineral phases of the ash were identified using an X-ray Diffractometer (XRD), while the mineral oxides were obtained using an X-ray Fluorescence Spectrometer. The AFT700 Furnace was used with its AFT700 software to evaluate the ash fusion temperatures of the ashes. The XRD patterns look similar, and quartz was found to be the dominant mineral phase present in the raw coal and bio-coal briquettes. The SiO2 (57–58%), Al2O3 (19–21%), and Fe2O3 (8–9%) were the major oxides observed in the ashes. The final fusion temperatures of the ashes range from 1300–1350 °C. The compositions of the ashes of the bio-coal briquettes are classified as detrital minerals. It was concluded that the addition of torrefied biomass (≤ 10%)and blended binder (le 15%) to coal gave a negligible impact on the ashes of the resultant bio-coal briquettes.

Enhanced photocatalytic decomposition of NO on portland cement concrete pavement using nano-TiO2 suspension

Photocatalyst titanium dioxide (TiO2) has been widely applied on asphalt and concrete pavements to mitigate the air pollution caused by traffic exhaust. In general, most of the TiO2 used in previous studies was pure anatase, which only exhibited excellent photocatalytic activity under ultraviolet (UV) light. Thus, N-doping method was selected to improve the photocatalytic activity, especially under visible light. Additionally, the TiO2 suspension was commonly used on the pavements comparing with other application methods. However, the Nano-TiO2 particles with great surface area-to-volume ratio and surface energy have a strong tendency to agglomerate in the suspension, which has significantly negative effects on the photocatalytic activity. Thus, the objective of this study was to enhance the photocatalytic performance of mortar specimens containing TiO2 by preparing optimum N-doped TiO2 and suspensions using both single-factor and orthogonal experimental design. Methylene blue (MB) decomposition results indicated that the optimum N-doped TiO2 was prepared with 1% N-dosage at 700 °C for 5 h. X-ray diffractometer (XRD) pattern results implied that the phase transformation from anatase to rutile occurred around 700–800 °C and anatase transferred to rutile completely at 900 °C. Absorbance results showed that the optimum suspension was prepared with following conditions: ultrasonic power 100 W, ultrasonic time 120 min, silica sol concentration 0.5%, and sodium hexametaphosphate (SHMP) dosage of 0.3%. Lastly, NO decomposition test was conducted to investigate the effects of TiO2 implementation methods and environmental factors on the photocatalytic performance of mortar specimens. The NO decomposition results showed that the optimum suspension could significantly improve the photocatalytic performance of specimens. Meanwhile, the NO decomposition percentage decreased with the increasing flow rate and NO concentration.

Structural, optical and photocatalytic properties of Ni doped BiFeO3 nanoparticles

This paper presents synthesis and study of Structural, Optical, and Photocatalytic properties of bismuth ferrite (BFO) and nickel doped bismuth ferrite (BiFe1-xNixO3) nanoparticles. The synthesis of BiFeO3 and BiFe1-xNixO3 (x = 0.02, 0.04) are done by Sol-Gel method. After synthesis the samples of pure and transition metal ion (Ni) doped bismuth ferrite have been studied by using X-ray diffractometer (XRD), X-ray Photoelectron spectroscopy (XPS), Field Emission Scanning Electron Microscope and Raman Spectroscopy. Optical properties are studied by using UV–vis spectroscopy using different wavelengths (range 300–800 nm). Photocatalytic properties are also studied by degradation of MB dye using prepared samples as photocatalyst. XRD patterns shows that all the prepared samples are crystalline and crystallinity increased by Ni-doping and shifts in XRD peaks by Ni-doping shows the distortion in the structure of BFO. Raman spectroscopy also indicates the rhombohedral distorted structure of Ni-doped BFO in R3C space group. FESEM micrographs shows that Ni-doped BFO has polyhedral and spherical shape grains and Ni doping cause reduction in grain size. Optical band gap reduced due to Ni-doping is shown by the UV–Vis spectroscopy results and Tauc’s plots. The increase in reduction of MB dye due to Ni-doping shows the enhanced photocatalytic properties of BFO by Ni doping.

Functional, structural and morphological property of green synthesized silver nanoparticles using azadirachta indica leaf extract

The development of a sustainable and environmentally friendly approach is necessary due to climate changes. The green synthesis method is the best alternative to prepare silver (Ag) nanoparticles, paying great attention due to the physical and chemical properties. In this study, Ag nanoparticles were synthesized from the leaf extracts of azadirachta indica (neem) at room temperature. The formation of silver nanoparticles was confirmed by Fourier transform infrared (FTIR) spectroscopy, X-ray diffractometer (XRD), and scanning electron microscopy (SEM) techniques. FTIR spectrum exhibits the reducing biomolecules within the plant leaf extract. The average crystalline size 57.04 nm was calculated using Debye’s Scherrer’s formula by the XRD pattern. SEM micrograph shows the spherical shape nanoparticles with less agglomerations.

High removal efficiency of tetracycline (TC) by biochar-supported zerovalent iron composite prepared by co-pyrolysis of hematite and pinewood

ABSTRACT There is a need to prepare a high-efficient sorbent to remove the recalcitrant tetracycline (TC) in wastewater. Herein, biochar-supported zerovalent iron (BC/ZVI) was fabricated in nitrogen ambience via one-step co-pyrolysis of hematite and pinewood. X-ray diffractometer pattern indicated pinewood catalyzed conversion of hematite to ZVI, which was otherwise transformed to FeO, Fe3O4 and ZVI without biomass. Batch sorption results indicated that TC removal capacities at pH 5 were 8.02, 177.70 and 301.39 mg g−1 by BC, ZVI and BC/ZVI, respectively. Overall, BC/ZVI showed excellent TC removal capacity through the complexation with Fe ions, surface adsorption and degradation. Thus, the agricultural and industrial wastes were converted via a one-step co-pyrolysis to a value-added product for highly efficient removal of TC in wastewater.

Synthesis and characterization of cadmium sulfide (CdS) thin films by cyclic voltammetry technique

Abstract Nanostructure (II-VI) semiconductor Cadmium Sulfide (CdS) have interesting due to their in scientific circle and varieties of encouraging potentials in extensive applications such as transparent windows, photoluminescence devices, sensors, solar cells, etc. In this work, nanocrystalline CdS thin films (TFs) synthesized on the Indium tin oxide (ITO) coated glass substrate via cyclic voltammetry (CV) with a three-electrode deposition technique. X-Ray Diffractometer (XRD) used for the structural study of TFs and the topographical image characterized by using an Atomic Force Microscope (AFM). XRD patterns of the TFs were shown that nanocrystaline in nature with a cubic structure at (2 0 0) as the preferential orientation. Chemical compositions of the deposited TFs analysed by using Fourier Transform Infrared Spectroscopy (FT-IR). The optical properties of CdS TFs characterized by using a UV–Vis spectrophotometer showed that the optical band gap energy (Eg) decreases from 2.92 eV to 2.28 eV with increasing of deposition time from 15 min to 60 min respectively. Urbach energy increases from 117 meV to 151 meV with increasing of deposition time from 15 min to 60 min respectively.

Terminalia catappa and carissa carandas assisted synthesis of Tio2 nanoparticles – A green synthesis approach

Nature motivates a researcher to carry out new research in science and technology, especially in the field of nanotechnology. In those natural systems, Terminalia Catappa and Carissa Carandas are one having a very significantly reducing and capping agent. The Present work focused on to synthesis of Titanium dioxide (TiO2) nanoparticles from Terminalia Catappa and Carissa Carandas plant extract using the Green synthesis method. The obtained TiO2 nanoparticles have been characterized by X-ray Diffractometer (XRD), Scanning Electron Microscopy (SEM), UV–Visible Spectroscopy (UV–Vis) and Fourier Transform Infrared Spectroscopy analysis. In the XRD pattern, the diffractogram indicates the formation of anatase phase TiO2 with the tetragonal crystal structure and the average crystalline size is roughly range as 10–21 nm. SEM micrograph reveals that the nanoparticles are homogeneously distributed with spherical shape morphology without agglomeration.

Biosynthesis of silver nanoparticle using flowers of Calotropis gigantea (L.) W.T. Aiton and activity against pathogenic bacteria

Silver nanoparticles (AgNPs) from silver nitrate solution are carried out using the flower extract of Calotropis gigantea. Silver nanoparticles were characterized by UV–vis spectrophotometer, X-Ray diffractometer (XRD). Reduction of silver ions in the aqueous solution of silver during the reaction was observed by UV–vis spectroscopy. Crystalline nature of synthesized silver nanoparticles was studied by XRD pattern, refraction peak using the Scherrer’s equation. Antibacterial activity of the silver nanoparticles was performed by disc diffusion method against Bacillus subtilis, Pseudomonas putida and Escherichia coli. The antibacterial activity of synthesized silver nanoparticles by flower extract of C. gigantea was found against B. subtilis (10 mm). Synthesised AgNPs has the efficient antibacterial activity against Gram positive bacteria.

Growth and Characterization of CZTS Thin Films Synthetized by Electrodeposition Method for Photovoltaic Applications

In the present work we deposited CZTS absorber material using a one-step electrodeposition method on ITO glass substrates. We studied the effect of sulfurization temperature on structural, morphological and optical properties of CZTS thin films sulfurized in N2+H2S atmosphere at 350, 375, 400 and 425°C for 10 min respectively for 10 min. The films have been charaterized by different techniques including X-ray diffractometer (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and UV-visible-NIR spectrophotometer. XRD patterns indicated kesterite CZTS with preferential orientation along (112) plane, the intensity of peaks increased with increase of sulfurization temperature signified the amelioration of the crystallinity with sulfurization temperature increased, the estimated crystallite size are in the range of 14.27-37.32 nm. Raman scattering experiments confirmed the presence of CZTS thin films by the characteristic peak at 336 cm−1. SEM images showed the morphology of CZTS thin films improved with increasing of sulfurization temperature. UV-Visible-NIR spectrophotometer showed that the values of optical absorption coefficient are larger than 104 cm−1 and optical band gap energy of CZTS thin films decreased with increasing of sulfurization temperature ranging 1.56 and 1.66 eV. These results make the electrodeposited CZTS films a suitable material as absorber material in solar cells applications based thin films.

Characterization of Cellulose Nanocrystals Derived from Umbrella Plant (Cyperus alternifolius Linn.)

Plant–based nanocrystals have gained wide research interest due to its application in nano–reinforcement. Hence, the study investigated the stems of umbrella plant as potentials source of cellulose fibers to synthesize cellulose nanocrystals (CNCs). The synthesis of CNCs were conducted using acid hydrolysis with 10 mL 64% w/w sulfuric acid for each gram of purified cellulose at 45°C for 30 min. The surface morphology, structural, physical and thermal properties of CNCs were characterized using field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), Fourier Transform Infrared spectroscopy (FTIR), X–ray diffractometer (XRD), and simultaneous thermal analyzer, respectively. The result showed that the CNCs were mixture of rod–like shape and spherical morphology. The CNC rods were less than 20 nm width and 200–300 nm length when viewed under FESEM. However, the CNC rods were shorter when viewed under TEM and had a width less than 5 nm and length between 20–50 nm. The spherical CNCs that were seen only under TEM were less than 20 nm in diameter. The FTIR spectra showed that the CNCs were composed of crystalline cellulose I wherein the molecular structure of cellulose was preserved after the hydrolysis. The XRD patterns showed that the CNCs were highly crystalline with crystallinity index value of 94.48%. Lastly, the CNCs exhibited a three–stage thermal decomposition behavior.

Structural, Microstructural, Electrical, and Magnetic Properties of CuFe2-(x+y)EuxScyO4 (where x and y vary from 0 to 0.03) Nanoparticles

In the present work, the CuFe2-(x+y)EuxScyO4 nanoparticles were prepared by solution combustion method for reporting the structural, microstructural, dielectric, and magnetic properties of prepared samples. The XRD (X-ray diffractometer) patterns confirm the spinel cubic structure with space group Fd3m. The average crystallite size was found in the range from 25 to 10 nm for x = y = 0.00, 0.01, 0.02, and 0.03 concentrations. The SEM (scanning electron microscopy) investigations indicate the porous nature and particle agglomeration. The elemental composition of the samples was studied by using energy-dispersive X-ray spectroscopy (EDS). The FTIR (Fourier transform-infrared spectroscopy) investigation shows the two absorption bands around 554.07 cm−1 and 468.98 cm−1 due to stretching vibrations of the Cu⟺O metal-oxygen bond at the A-site and stretching vibrations of Fe⟺O metal-oxygen bond at the B-site, respectively. The real and imaginary parts of dielectric constant, dielectric loss tangent, AC conductivity, and impedance spectroscopy have been recorded by the methods of impedance analyzer from the range 0.1 KHz to 1 MHz. The dielectric constant and dielectric loss show maximum value at smaller frequency region and are decreases with increase in frequency. AC conductivity increases with the increase of frequency. The real and imaginary part of impedance spectra as function of frequency was studied. The Cole-Cole plots drawn from the impedance spectra show one semicircle for each of the samples. The magnetic hysteresis loop reveals the soft ferromagnetic nature. The magnetic parameters such as saturation magnetization, coercivity, and remanence magnetization decrease with the increase of Eu3+ and Sc3+ concentration.

Preparation and properties of hot-deformed magnets processed from nanocrystalline/amorphous Nd–Fe–B powders

The hot-deformed magnets processed from nanocrystalline/amorphous Nd–Fe–B powders were prepared under different hot-pressing temperatures (600–750 °C, at intervals of 25 °C) by the self-made hot-pressing equipment. The microstructure and magnetic properties of hot-deformed magnets prepared at different temperatures were also investigated. When the temperature is above 650 °C, the density of magnet reaches 7.5 g·cm−3. The optimum magnetic properties of magnetic induction intensity of Br = 1.3 T, optimum energy product of (BH)max = 282.5 kJ·m−3, intrinsic coercivity of Hcj = 1130.0 kA·m−1 of hot-deformed magnets are obtained at hot-pressing temperature of 650 °C. X-ray diffractometer pattern shows that the (00L) texture has been obtained. For the microstructural characteristic, on the one hand, the good magnetic performance is attributed to the fine platelet-like grains with an average length of 410–440 nm at the hot-pressing temperature range from 625 to 675 °C. On the other hand, the unaligned coarse grains are observed in all the samples. And the areal fraction of those is gradually increasing with the rise of the hot-pressing temperature, which tends to deteriorate the magnetic properties. The composition map shows the accumulation of Nd/Pr-rich phase in the coarse grains’ region.

Performance evaluation of highly active and novel La0.7Sr0.3Ti0.1Fe0.6Ni0.3O3-δ material both as cathode and anode for intermediate-temperature symmetrical solid oxide fuel cell

In comparison to various power generating devices/energy conversion systems, solid oxide fuel cell (SOFC) has received much attention due to its remarkable efficiency, reliability and low pollution. Modified pechini method is used to synthesize La0.7Sr0.3Ti0.1Fe0.6Ni0.3O3-δ (LSTFN) perovskite material and is utilized as cathode and anode for intermediate-temperature symmetrical solid oxide fuel cell (IT-SSOFC). The X-ray diffractometer (XRD) patterns reveals perovskite cubic structure with single phase for LSTFN. The maximum conductivity ~318 Scm−1 is obtained for LSTFN in air at a temperature of 700 °C, but is decreased with further increase in temperature due to small polaron mechanism. However, the conductivity is enhanced up to ~1.1 Scm−1 at the same temperature in the presence of dry H2, being capable to be utilized both as anode and cathode. Low polarization resistance (Rp) ~0.047 (with air) and 0.201Ωcm2 (with dry H2) is exhibited by as prepared perovskite material at a temperature of 800 °C. The fabricated symmetrical cell maintains good stability with no apparent degradation during the tested hours ~300 in air and ~100 with dry H2.

Study of the microstructure and crystal orientation of as-cast Ti-10.2Mo-19.5Nb alloy

Ti-based alloys particularly metastable β-type Ti alloys have been attracting an increasing attention as crucial biomedical materials in the past few decades due to their moderate strength, good corrosion resistance, good biocompatibility, low elastic modulus and high ductility. This work is aimed at studying the microstructural evolution and the crystal orientation of metastable β-type Ti-Mo-Nb alloy designed using the MoEq, d-electron theory and e/a ratio approaches. This is a preliminary study on the thermo-mechanical processing of the designed alloy, which could produce alloys with lower elastic modulus (≈ 35 GPa) when all the β phase have the same planar orientation. The optical microscopy (OM) was used to perform microstructural analysis while the electron backscatter diffractometer (EBSD) was utilized for the crystal orientation. Also, Phase identification was conducted using the X-ray diffractometer (XRD). Results show that the EBSD microstructure of as-cast Ti-10.2Mo-19.5Nb alloy revealed the presence of orthorhombic martensitic α phase precipitates in the β phase matrix. However, no orthorhombic martensitic α phase was observed in the optical micrograph and the XRD pattern. Furthermore, no precipitates of ω phase was revealed by the three analytical techniques, probably due to its small size (nm) in the alloy. The crystal orientation was random. In as-cast condition, this alloy has shown a lower elastic modulus than those of the conventional orthopaedic implant materials including Ti6Al4V (110 GPa), CoCr (220 GPa) and 316L stainless steel (205 GPa).

Metal organic frameworks of lanthanum and iron using BDC linker as catalysts for glucose conversion into 5-hydroxymethylfurfural (5-HMF)

Lanthanum and Iron-Metal Organic Frameworks (La-MOFs, Fe-MOFs) have been successfully synthesized through solvothermal method and applied as catalysts to convert glucose into 5-Hydroxymethylfurfural (5-HMF). 5-HMF is a very promising energy source which extensively used in chemical industries and polymer materials. MOF is used as source of Lewis and Brønsted acid that can improve the conformation of 5-HMF in glucose transformation. The XRD pattern, surface morphology, chemical composition, absorption spectra, and surface area were characterized by X-Ray Diffractometer (XRD), Scanning Electron Microscopy-Energy Dispersive X-Ray (SEM-EDX), Fourier Transform Infrared (FTIR) and Brunauer-Emmelt-Tellers (BET). The specific peaks of La-MOF on XRD pattern corresponded at 2θ = 8° respectively, while Fe-MOF corresponded to MIL-88B structure at 2θ = 9°. SEM analysis of La-MOF and Fe-MOF revealed the catalysts morphology were rod-like and rhombic. The FTIR spectrum of La-MOF showed the broadening peak at 3526 cm−1 for O-H stretching vibrations while Fe-MOF had sharp peak intensity at 749 cm−1 for C-H bending vibrations. The surface area of the La-MOF and Fe-MOF were 107.107 m2/g and 215.435 m2/g, respectively. The activity of La-MOF and Fe-MOF as catalysts was performed in 10 mL vial glass reactor at T = 403 K with varied time from 0–8 h and catalyst loading were varied from 8–12 mg. The product analysis was carried out using High Performance Liquid Chromatography (HPLC) in which Fe-MOF showed higher activity giving yield 26.79 % rather than La-MOF with 19.2 % yield of 5-HMF in 6 h reaction time using 10 mg catalyst in DMSO as solvent.

Synthesis, Characterization and Bioactivity of Fluoride Containing Borosilicate Glass Matrix Composite

Fluoride containing borosilicates find interesting applications in biomedical transplants and dentistry, wherein calcium and magnesium play pivotal role in human bone formation. In the present work, calcium and magnesium fluoride containing borosilicate glass matrix composites were synthesized via sol-gel route. The as synthesized and heat-treated samples were characterized using various techniques such as X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FT-IR), and thermogravimetric analysis (TGA). and Scanning Electron Microscopy-Energy dispersive spectroscopy (SEM-EDS). The samples were stabilized at suitable temperature based on the thermogravimetric analysis (TGA). The XRD patterns of as prepared samples showed various crystalline phases with varied degree of crystallinity. Heat-treated samples were tested for their in–vitro bioactivity. Interaction at sample-SBF interface was investigated by dipping the samples in simulated body fluid (SBF) at 37 °C. The analysis of the samples dipped in SBF and that of the residual SBF was carried out using various characterization techniques. Increasing the ageing time, the samples exhibited better in-vitro bioactivity.