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J.H. Kim and J.-H. Lee

Abstract

In order to fabricate graphite nanosheets from graphite flakes, edge-functionalized graphite nanosheets were prepared by a functionalization method using phthalic acid as the molecule to be grafted. A polyphosphoric acid/P2O5 solution containing graphite and phthalic acid were heated at different temperatures for 72 h in a nitrogen atmosphere. It was confirmed by transmission electron microscopy and atomic force microscopy that the resultant phthalic acid-functionalized graphite nanosheets had a large surface area of 20.69 μm2 in average and an average thickness of 1.39 nm. It was also found by X-ray diffractometry and Fourier transform infrared spectroscopy (FT-IR) analysis that the functionalization caused the formation of C=O bonds at the edges of the graphite nanosheets. The yield from this functionalization method was found to be dependent on the reaction temperature, only when it is between 70 and 130°C, because of the dehydration of phthalic acid at higher temperatures. This was confirmed by FT-IR analysis and the observation of low thermal energies at low temperatures.

Open access

Talat Zeeshan, Safia Anjum, Hina Iqbal and Rehana Zia

Abstract

A series of copper substituted cobalt chromium ferrites, CuxCo1 - xCr0.5Fe1.5O4 (x = 0, 0.2, 0.4, 0.6, 0.8, 1.0) has been synthesized, by employing powder metallurgy method. Calcination of the samples has been carried out for 24 hours at 1100 °C. The resultant materials have been investigated by using a variety of techniques, including X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM)), scanning electron microscopy (SEM), and ultraviolet visible spectroscopy (UV-Vis). The XRD patterns confirmed that all compositions had a cubic spinel structure with a single phase and the lattice parameter was found to increase with increasing copper concentration. FT-IR spectroscopy has been used for studying the chemical bonds in the spinel ferrite. Shifting of the bands ν1 and ν2 has been observed. It has been revealed from VSM analysis that saturation magnetization and coercivity decrease with rising the Cu+2 doping. Magnetic properties have been explained on the basis of cation distribution. Scanning electron microscopy (SEM) has been used to study the surface morphology of prepared samples. UV-Vis analysis revealed the optical absorption of the samples. An increase in band gaps has been observed with increasing copper concentration in the sample.

Open access

M.R. Jagadeesh, H .M. Suresh Kumar and R. Ananda Kumari

Abstract

A new semi-organic non linear optical crystal, L-leucine phthalic acid potassium iodide (LLPPI) has been grown from an aqueous solution by slow evaporation method. The grown crystals were subjected to different characterizations, such as single crystal XRD, FT-IR, UV-Vis, TGA, SEM, EDAX, micro hardness, dielectric and powder SHG. Single crystal structure was determined from X-ray diffraction data and it revealed that the crystal belongs to triclinic system with the space group P1. The vibrational frequencies of various functional groups were derived from FT-IR spectrum. Thermal stability of the grown crystal was investigated by TG-DTA studies and it was observed that the crystal was thermally stable up to 192 °C. Optical absorption study was carried out and a good transparency in the entire visible region was observed at the lower cutoff wavelength of 227 nm. Dielectric study was performed as a function of frequency and normal dielectric behavior was observed. The micro hardness test was carried out and the load dependent hardness was measured. Kurtz powder method was employed to explore the NLO characteristics of the grown crystal.

Open access

Kais Elghniji, Mohamed Saad, Manel Araissi, Elimame Elaloui and Younes Moussaoui

Abstract

Two titanium phosphate materials (TpP and ThP) have been successfully synthesized by sol-gel route with controlled precipitation and hydrolysis. The TpP material was obtained from the reaction between precipitated titania and phosphate buffer solution H2PO4− /HPO42− (pH = 7.3). The TpP material was prepared through hydrolysis of titanium in the presence of H2PO4−/HPO42. The probable state of the phosphate anions in titania framework and their effect on the anatase-to-rutile transformation were characterized by ICP-AES, DTA-TG, 31P NMR, FT-IR, and Raman analysis HRTEM/SEM. FT-IR and 31P NMR analyses of titanium phosphate TpP calcined at low temperature showed that the phosphate species existed not only as Ti-O-P in the bulk TiO2 but also as amorphous titanium phosphates, including bidentate Ti(HPO4)2 and monodentate Ti(H2PO4)4. Increased calcination temperature only gave an enrichment of bidentate structure on the titania surface. For the TpP material, H2PO4−/HPO42− anions were introduced into the initial solution, before precipitation, what promoted their lattice localization. At high temperatures, all the phosphorus inside the bulk of TiO2 migrated to the surface. The Raman analysis of both samples showed that the bidentate phosphates increased the temperature of the anatase-to-rutile phase transformation to more than 1000 °C with the formation of well crystalline TiP2O7 phase. This phenomenon was more evident for TpP sample.

Open access

Ali N. Siyal, Saima Q. Memon and M.Y. Khuhawar

Abstract

An attempt has been made to recycle Styrofoam waste to a novel functional polymer, Phenyl thiosemicarbazone surface (PTS). Polystyrene (PS) obtained from Styrofoam waste was acetylated and then condensed to PTS by reacting it with 4-Phenyl-3-thiosemicarbazide ligand and characterized by FT-IR spectroscopy and elemental analysis. Synthesized PTS was applied successfully for the treatment of lead contaminated water by batch extraction method. Sorption variables were optimized (pH 8, adsorbent dose 53mg, initial Pb(II) ion concentration 10mgl-1 and agitation time 90min) by factorial design approach. Lead uptake by PTS was found much sensitive to the pH of Pb(II) ion solution. The maximum removal (99.61%) of Pb(II) ions was achieved at optimum conditions. The Langmuir and D-R isotherm study suggested the monolayer, favorable (RL=0.0001-0.01) and chemisorption (E=20.41±0.12kJmol-1) nature of the adsorption process. The sorption capacity of PTS was found to be 45.25±0.69mgg-1. The FT-IR spectroscopy study showed the involvement of nitrogen and sulphur of thiosemicarbazone moiety of PTS for the uptake of Pb(II) ions by five membered chelate formation.

Open access

Yufeng Ma, Xiang Geng, Xi Zhang, Chunpeng Wang and Fuxiang Chu

Abstract

A novel 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) graft γ-amino propyl triethoxy silane (KH550) was synthesized and introduced on the surface of wood fiber. Finally DOPO-g-KH550 treated wood fiber (DKTWF) was used to prepare DKTWF composite phenolic foams (DKTWFCPF). The structures of DOPO-g- KH550 was acknowledged by Fourier transform infrared (FT-IR) and nuclear magnetic resonance (1H-NMR). The structures of DKTWF were confirmed by FT-IR. Compared with wood fiber, the diffraction peaks’ position was basically unchanged, but the crystallinity was slightly increased and thermal stability were dramatically improved, T5% and Tmax increased by 21.9o and 36.1o respectively. But the char yield (800o) was slightly reduced. With the dosage of DKWF, there were different degrees of improvement including the mechanical properties, flame retardancy and microstructure of DKTWFCPF. Comprehensive analysis, the interfacial compatibility was significantly improved between DKTWF and phenolic resin, and the suitable content of DKTWF was 4%.

Open access

Anu Dhupar, Suresh Kumar, Vandana Sharma and J.K. Sharma

Abstract

In the present work, mixed structure Zn(S,O) nanoparticles have been synthesized using solution based chemical coprecipitation technique. Two different zinc sources (Zn(CH3COO)2·2H2O and ZnSO4·7H2O) and one sulfur source (CSNH2NH2) have been used as primary chemical precursors for the synthesis of the nanoparticles in the presence and absence of a capping agent (EDTA). The structural, morphological, compositional and optical properties of the nanoparticles have been analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transmission infra-red (FT-IR) and UV-Visible (UV-Vis) spectroscopy. XRD revealed the formation of mixed phases of c-ZnS, h-ZnS and h-ZnO in the synthesized nanoparticles. The surface morphology was analyzed from SEM micrographs which showed noticeable changes due to the effect of EDTA. EDX analysis confirmed the presence of zinc, sulfur and oxygen in Zn(S,O) nanoparticles. FT-IR spectra identified the presence of characteristic absorption peaks of ZnS and ZnO along with other functional group elements. The optical band gap values were found to vary from 4.16 eV to 4.40 eV for Zn(S,O) nanoparticles which are higher in comparison to the band gap values of bulk ZnS and ZnO. These higher band gap values may be attributed to the mixed structure of Zn(S,O) nanoparticles.

Open access

B. Grabowska, K. Kaczmarska, A. Bobrowski, Ż. Kurleto-Kozioł and Ł. Szymański

Abstract

The spectroscopic FT-IR and FT-Raman methods allowed to identify the cross-linking process of the aqueous composition of poly(acrylic acid)/sodium salt of carboxymethyl starch (PAA/CMS-Na) applied as a binder for moulding sands (as a novel group binders BioCo). The cross-linking was performed by physical agent, applying the UV-radiation. The results of structural studies (IR, Raman) confirm the overlapping of the process of cross-linking polymer composition PAA/CMS-Na in UV radiation. Taking into account the ingredients and structure of the polymeric composition can also refer to a curing process in a binder - mineral matrix mixture. In the system of binder-mineral matrix under the influence of ultraviolet radiation is also observed effect of binding. However, the bonding process does not occur in the entire volume of the investigated system, but only on the surface, which gives some possibilities for application in the use of UV curing surface of cores, and also to cure sand moulds in 3D printing technology.

Open access

Nashiruddin Ahammed, Md Samim Hassan and Mehedi Hassan

Abstract

In this research article, pure and 1 %, 3 % and 5 % aluminium doped zinc oxide nanoparticles (NPs) were prepared via sol-gel method and then calcined at 500 °C. X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transform infrared (FT-IR) spectroscopy, UV-Vis spectroscopy, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) techniques were used to investigate the structural, optical and thermal properties of synthesized pure and Al doped ZnO nanoparticles. Energy dispersive X-ray spectroscopy (EDX) analysis revealed high purity of nanoparticles in the synthesized products without any impurity peaks. Mean dimension of the nanoparticles was ~28 nm and they were hexagonal in shape, according to the images analyzed by transmission electron microscope (TEM). The optical absorption spectra of pure and Al doped ZnO samples studied using UV-Vis spectrometry have been presented and we have observed that the band gap increases with increasing Al concentration. In FT-IR spectra, the broad absorption peaks around 485 cm−1 and 670 cm−1 were assigned to Zn–O vibration. Above 450 °C, the TG curve became flat what means there was no weight loss. In the DSC curve it is seen that the transition at 150 °C was highly exothermic because of structural relaxation and on doping the exothermic peaks became shifted to the lower value of temperature. These types of materials are very useful in optoelectronics applications.

Open access

Surendra Singh, Anshuman Sahai, S.C. Katyal and Navendu Goswami

Abstract

We have synthesized zinc-copper ferrite (ZCFO) employing exploding wire technique (EWT). The X-ray diffraction (XRD) data confirm the formation of single phase spinel ZCFO, which is in good agreement with Fourier transform infrared spectroscopy (FT-IR), UV-Vis, and Raman spectroscopic analyses. It is also clearly seen in the SEM micrographs that the grains in ZCFO ferrite are very rough, which allows adsorption of gas like oxygen and therefore, the material can behave as active sensing surface. The size range of the grains in prepared sample is of 200 nm to 500 nm. The FT-IR spectrum of the nanocomposite consists of two broad bands, one at 580.4 cm−1 due to M–O stretching mode at the tetrahedral site and the other at 400.7 cm−1 due to M–O stretching mode at the octahedral site. The nanoparticles show a UV-Vis absorption band in the wavelength region of 400 nm to 700 nm. The energy band gap for the prepared nanomaterial was estimated to be 3.16 eV. Thus, the ferrite nanocomposite prepared by EWT is optically active. According to present literature, Raman spectroscopy study on zinc-copper ferrite system has not been reported till date. By suitable attributing various Raman modes, we have further confirmed the formation of ZCFO nanophase through the present novel approach.