Spectral,X-ray diffraction,surface morphological and thermal studies of gamma-irradiated potassium bis(oxalato)zincate(II)dihydrate

ABSTRACT

Potassium bis(oxalato)zincate(II)dihydrate was prepared and characterized. The sample was irradiated with ⁶⁰Co gamma rays up to 900?kGy. Infrared, Raman and photoluminescence spectra, X-ray diffraction pattern, surface morphology by AFM and SEM and non-isothermal decomposition of the complex were studied before and after irradiation. Spectral studies suggested significant radiation damage. X-ray diffraction studies showed reduction in unit cell volume and average crystallite size. Both unirradiated and irradiated samples of the complex belong to the hexagonal crystal system. Surface morphology of the complex changed upon irradiation. Thermal decomposition was enhanced.     

A study of the effect of gamma and laser irradiation on the thermal,optical and structural properties of CR-39 nuclear track detector

A comparative study of the effect of gamma and laser irradiation on the thermal, optical and structural properties of the CR-39 diglycol carbonate solid state nuclear track detector has been carried out. Samples from CR-39 polymer were classified into two main groups: the first group was irradiated by gamma rays with doses at levels between 20 and 300 kGy, whereas the second group was exposed to infrared laser radiation with energy fluences at levels between 0.71 and 8.53 J/cm². Non-isothermal studies were carried out using thermogravimetry, differential thermogravimetry and differential thermal analysis to obtain activation energy of decomposition and transition temperatures for the non-irradiated and all irradiated CR-39 samples. In addition, optical and structural property studies were performed on non-irradiated and irradiated CR-39 samples using refractive index and X-ray diffraction measurements. Variation in the onset temperature of decomposition T _o, activation energy of decomposition E _a, melting temperature T _m, refractive index n and the mass fraction of the amorphous phase after gamma and laser irradiation were studied.

It was found that many changes in the thermal, optical and structural properties of the CR-39 polymer could be produced by gamma irradiation via degradation and cross-linking mechanisms. Also, the gamma dose has an advantage of increasing the correlation between thermal stability of the CR-39 polymer and bond formation created by the ionizing effect of gamma radiation. On the other hand, higher laser-energy fluences in the range 4.27–8.53 J/cm² decrease the melting temperature of the CR-39 polymer and this is most suitable for applications requiring molding of the polymer at lower temperatures.     

Ion-Polymer Interactions in SmCl3(H2O)6 Doped Poly(ethylene oxide) Electrolytes

Pure and SmCl₃(H₂O)₆ doped poly(ethylene oxide) (PEO) samples were prepared using a solvent casting method. These samples were characterized using Fourier transform infrared (FTIR), X-ray diffraction (XRD), and differential scanning colorimetry (DSC) techniques. The FTIR spectra indicate that, only at low dopant concentrations, the interactions between Sm³⁺ and ether oxygen atoms in PEO are dominant. As the dopant concentration increases, these interactions result in the formation of dopant aggregates or agglomerates leading to a phase separation into a polymer-rich phase and a dopant-rich phase in the films, which have been confirmed by XRD and DSC results.     

Effect of ion beam irradiation on palladium (II) acetyl acetonate dispersed in polymer matrix

Composites, containing different concentrations of palladium (II) acetylacetonate in polymethyl methacrylate (PMMA) matrix were prepared by vigorous mixing. PMMA was prepared by solution polymerization technique. The composites were irradiated with a 120 MeV Ni¹⁰⁺ beam at two different fluences of 1×10¹¹ and 5×10¹² ions/cm² to study ion-induced effects on their dielectric, structural properties and surface morphology. AC electrical properties of these samples were studied in the frequency range 100 Hz to 10 MHz. The dielectric permittivity/loss shows frequency dependent behavior and it obeys the universal law of dielectric (i.e. ?α f ^n?1) for pristine and irradiated samples at high frequency. The crystalline size and crystallinity of the composites were studied by X-ray diffraction analysis. Decrease in peak intensity after irradiation signifies the amorphization which is also responsible for decrease in T _g as obtained by means of differential scanning calorimetry measurement. Fourier transform infrared spectra also support this result. Surface roughness increases upon irradiation as observed from scanning electron microscopy.     

The study of gamma irradiation effects on poly (glycolic acid)

We have investigated the effects of gamma irradiation on chemical structure, thermal and morphological properties of biodegradable semi-crystalline poly (glycolic acid) (PGA). PGA samples were subjected to irradiation treatment using a ⁶⁰Co gamma source with a delivered dose of 30, 60 and 90?kGy, respectively. Gamma irradiation induces cleavage of PGA main chains forming ～O?H₂ and ?H₂COO～ radicals in both amorphous and crystalline regions. The free radicals formed in the amorphous region abstract atmospheric oxygen and convert them to peroxy radicals. The peroxy radical causes chain scission at the crystal interface through hydrogen abstraction from methylene groups forming the ～?HCOO～ (I) radical. Consequently, the observed electron spin resonance (ESR) doublet of irradiated PGA is assigned to (I). The disappearance of the ESR signal above 190°C indicates that free radicals are formed in the amorphous region and decay below the melting temperature of PGA. Fourier transform infrared and optical absorption studies confirm that the groups are not influenced by gamma irradiation. Differential scanning calorimetry (DSC) studies showed that the melting temperature of PGA decreased from 212°C to 202°C upon irradiation. Degree of crystallinity increased initially and then decreased with an increase in radiation as per DSC and X-ray diffraction studies. Irradiation produced changes in the physical properties of PGA as well as affecting the morphology of the material.     

Effect of electron beam irradiation on the structural,thermal and optical properties of poly(vinyl alcohol) thin film

Poly(vinyl alcohol) (PVA) polymer was prepared using the casting technique. The obtained PVA thin films have been irradiated with electron beam doses ranging from 20 to 300 kGy. The resultant effect of electron beam irradiation on the structural properties of PVA has been investigated using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR), while the thermal properties have been investigated using thermo-gravimetric analysis and differential thermal analysis (DTA). The onset temperature of decomposition T ₀ and activation energy of thermal decomposition E _a were calculated, results indicate that the PVA thin film decomposes in one main weight loss stage. Also, the electron beam irradiation in dose range 95–210 kGy led to a more compact structure of the PVA polymer, which resulted in an improvement in its thermal stability with an increase in the activation energy of thermal decomposition. The variation of transition temperatures with electron beam dose has been determined using DTA. The PVA thermograms were characterized by the appearance of an endothermic peak due to melting. In addition, the transmission of the PVA samples and any color changes were studied. The color intensity Δ E was greatly increased with increasing electron beam dose, and was accompanied by a significant increase in the blue color component.     

Electron induced modification in poly(ethylene terephthalate)

Abstract

The effect of 100 kGy dose of 2 MeV electron irradiation on Poly(ethylene terepthalate) (PET) has been studied by different characterisation techniques such as the Fourier transformed IR spectroscopy, electron spin resonance spectroscopy, thermogravimetric analysis, differential scanning calorimetry and X-ray diffraction analysis. Oxidative degradation leading to amorphisation of the polymer has been observed from spectral analysis. The thermal stability of the polymer was found to decrease due to electron irradiation. The thermal decomposition temperature as well as the melting temperature in case of irradiated PET was found to be decreased due to electron bombardment. A decrease in crystallinity of the polymer has also been observed after irradiation.     

Magnetic Study of Nanocrystalline Ferrites and the Effect of Swift Heavy Ion Irradiation

100 MeV Si⁺⁷ irradiation induced modifications in the structural and magnetic properties of Mg_0.95Mn_0.05Fe₂O₄ nanoparticles have been studied by using X-ray diffraction, Mössbauer spectroscopy and a SQUID magnetometer. The X-ray diffraction patterns indicate the presence of single-phase cubic spinel structure of the samples. The particle size was estimated from the broadened (311) X-ray diffraction peak using the well-known Scherrer equation. The milling process reduced the average particle size to the nanometer range. After irradiation a slight increase in the particle size was observed. With the room temperature Mössbauer spectroscopy, superparamagnetic relaxation effects were observed in the pristine as well as in the irradiated samples. No appreciable changes were observed in the room temperature Mössbauer spectra after ion irradiation. Mössbauer spectroscopy performed on a 12 h milled pristine sample (6 nm) confirmed the transition to a magnetically ordered state for temperatures less than 140 K. All the samples showed well-defined magnetic ordering at 5 K, whereas, at room temperature they were in a superparamagnetic state. From the magnetization studies performed on the irradiated samples, it was concluded that the saturation magnetization was enhanced. This was explained on the basis of SHI irradiation induced modifications in surface states of the nanoparticles.     

Sonochemical effect on two new Ruthenium(II) complexes with ligand (E)-N-((6-bromopyridin-2-yl)methylene)-4-(methylthio)aniline precursors for synthesis of RuO2 nanoparticles

Two novel Ru(II) complexes [(η⁶-p-cymene)RuCl(L2)]PF₆ (R2) and [(η⁶-C₆H₆)RuCl(L2)]PF₆ (R4), with ligand (E)-N-((6-bromopyridin-2-yl)methylene)-4-(methylthio)aniline (L2), were synthesized and characterized by elemental analysis, ¹H NMR, ¹³C NMR and IR spectroscopy. Based on X-ray crystallography studies, complexes R2 and R4 have coordination environments with formulated (η⁶-p-cymene)Ru(N₂Cl) and (η⁶-C₆H₆)Ru(N₂Cl), respectively. The thermal stabilities of compounds R2 and R4 were studied by thermal gravimetric (TG) and differential scanning calorimetry (DSC). Thermal decomposition of these complexes was at 280 °C and 260 °C under air atmosphere respectively. The interaction of these complexes with calf thymus DNA (CT-DNA) was explored through electronic absorption spectra, fluorescence and redox behavior studies. The results showed that the complexes bind to CT-DNA with electrostatic interactions. Nanoparticles of RuO₂ were prepared by calcination of R2 and R4. Also the role of the ultrasound waves on the characteristics of the RuO₂ nanoparticles was studied. The nanoparticles were characterized by IR spectroscopy and X-ray diffraction (XRD). Also size and morphology of nanoparticles were studied by scanning electron microscopy (SEM).     

Microstructure change in poly(ethersulfone) films by swift heavy ions

PES membrane of thickness 25 μm was irradiated by Cl⁹⁺ ions of energy 100 MeV at IUAC, New Delhi. Microstructure changes due to exposure to high-energy ions were investigated by Fourier transform infrared (FTIR) and ultraviolet/visible (UV/vis) absorption spectroscopies, X-ray diffraction technique and by dynamic mechanical analysis (DMA). A significant loss of crystallinity is observed by the XRD data. Particle size or grain size calculated using Scherrer formula indicates measurable change in particle size of irradiated samples. The polymer chain scissions and structure degradations are expected to occur for irradiated samples. Optical properties of the films were changed due to irradiation that could be clearly seen in the absorption spectra. FTIR does not show the remarkable change in the irradiated samples, but there is some change in the surface roughness observed by AFM.     

Optical characteristics of amorphous V2O5 thin films colored by an excimer laser

The V₂O₅ films were prepared by an RF sputtering method, and the amorphous films were colored by an UV excimer laser. The crystallinity of the as-grown V₂O₅ film was degenerated greatly by laser irradiation, as determined by X-ray diffraction (XRD) and Raman studies. The transmission and complex refractive index spectra of the V₂O₅ film were affected by variations in the microstructure, including the surface morphology, crystalline structure, and substoichiometry with an oxygen deficiency. Considerable emissions due to oxygen vacancies and band transition of photoluminescence (PL) peaks were observed, and the peaks were significantly changed after laser irradiation. The variations in the optical properties in both films may be attributed to oxygen deficiency induced by laser irradiation.     

Facile synthesis and capacitive performance of the Co(OH)2 nanostructure via a ball-milling method

Co(OH)₂ nanoparticles were synthesized using only CoSO₄·7H₂O and NaOH as reactants without other auxiliary reagents via a simple, low-cost and practical ball-milling technique and investigated as the active electrode materials for supercapacitors. The structure and morphology of the resulting Co(OH)₂ samples were examined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and transmission electron microscopy (TEM). The observations revealed the formation of brucite-like phase of β-Co(OH)₂, which had an irregular sphere-like shape with an average size of 50-100 nm. When investigated as electrode materials for supercapacitors, the β-Co(OH)₂ exhibited good energy-storage performances in terms of high specific capacitance of 599 F g⁻¹ and excellent capacity retention, suggesting its potential application in the electrode material for supercapacitors.     

Structural transformations preparing the dehydration of Ca(OH)2

The mechanism of the thermal decomposition of earth alkaline hydroxides has been extensively studied (Niepce, 1976). It results from the formation of water molecules preceding the decomposition. Prereactional effects have been evidenced by different experimental techniques, in a large temperature range before the dehydration temperature (570 K with P_H2O = 1.73 torr) (Freund and Wengeler, 1980; Freund, Scheikh-Ol-Eslami and Gentsch, 1975). In particular, X-ray and neutron diffraction studies on powders and single crystals of Ca(OH)₂ and Ca(OD)₂ have already revealed structural discontinuities at different temperatures which depend on the water pressure conditons (Chaix-Pluchery, 1986; Chaix-Pluchery, Bouillot, Ciosmak, Niepce and Freund, 1983; Chaix-Pluchery, Pannetier, Bouillot and Niepce, 1987).     

Chemical synthesis of spinel nickel ferrite (NiFe2O4) nano-sheets

The present investigation is related to the deposition of single-phase nano-sheets spinel nickel ferrite (NiFe₂O₄) thin films onto glass substrates using a chemical method. Nano-sheets nickel ferrite films were deposited from an alkaline bath containing Ni²⁺ and Fe²⁺ ions. The films were characterized for their structural, surface morphological and electrical properties by means of X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and two-point probe electrical resistivity techniques. The X-ray diffraction pattern showed that NiFe₂O₄ nano-sheets are oriented along (3 1 1) plane. The FT-IR spectra of NiFe₂O₄ films showed strong absorption peaks around 600 and 400 cm⁻¹ which are typical for cubic spinel crystal structure. Microstructural study of NiFe₂O₄ film revealed nano-sheet like morphology with average sheet thickness of 30 nm. The room temperature electrical resistivity of the NiFe₂O₄ nano-sheets was 10⁷ Ω cm.     

Effect of 100 MeV O7+ ion beam irradiation on structural,optical and electronic properties of SnO2 thin films

In this paper, we present the impact of swift heavy ion beam irradiation on the structural, optical and electronic properties of SnO₂ thin films. Thin films were deposited using the pulsed laser deposition technique on Al₂O₃ substrates. Atomic force microscopy, X-ray diffraction, UV–visible absorption and temperature-dependent resistivity measurements were performed to explore the morphological, structural, optical and electronic properties of the as-deposited and irradiated samples. The peak intensity of the (200) peak was found to decrease monotonously with increasing irradiation fluence. The band gap energy of the 1×10¹¹ ion/cm² irradiated sample was found to increase. The electrical resistivity of the samples showed a continuous increase with the irradiation fluence.     

Effect of 50 MeV Li+3 and 80 MeV C+5 ions’ beam irradiation on the optical,structural, chemical and surface topographic properties of PMMA films*

The self-standing films of polymethyl methacrylate (PMMA) were irradiated under vacuum with 50?MeV lithium (Li³⁺) and 80?MeV carbon (C⁵⁺) ions to the fluences of 3?×?10¹⁴, 1?×?10¹⁵, 1?×?10¹⁶ and 1?×?10¹⁷ ions µm^?2. The pristine and irradiated samples of PMMA films were studied by using ultraviolet–visible (UV–Vis) spectrophotometry, Fourier transform infrared, X-ray diffractrometer and atomic force microscopy. With increasing ion fluence of swift heavy ion (SHI), PMMA suffers degradation, UV–Vis spectra show a shift in the absorption band from the UV towards visible, attributing the formation of the modified system of bonds. E_g and E_a decrease with increasing ion fluence. The size of crystallite and crystallinity percentage decreases with increasing ion fluence. With SHI irradiation, the intensity of IR bands and characteristic bands of different functional groups are found to shift drastically. The change in (E_g) and (N) in carbon cluster is calculated. Shifting of the absorption band from the UV towards visible along with optical activity and as a result of irradiation, some defects are created in the polymer causing the formation of conjugated bonds and carbon clusters in the polymer, which in turn lead to the modification in optical properties that could be useful in the fabrication of optoelectronic devices, gas sensing, electromagnetic shielding and drug delivery.     

热处理对CuIn(S,Se)2薄膜断面成分均匀性的影响

用同时硒硫化共溅射Cu-In预制层的方法制备了CuIn(S,Se)₂薄膜．为了了解热处理对CuIn(S,Se)₂薄膜断面成分均匀性的影响,对经"一段式"热处理(500 ℃)和"二段式"热处理(250 ℃保温然后500 ℃)的样品进行了研究．XRD测试结果表明,经过"一段式"热处理后的样品XRD(112)峰出现劈裂现象,而经过"二段式"热处理的样品XRD(112)峰比较匀称．GIXRD和EDS测试证明样品经过"二段式"热处理后断面成分均匀性较好．通过XRD 和Raman测试对两种热处理下的反应机理进行了研究,阐述了两种热处理对CuIn(S,Se)₂薄膜断面成分均匀性的影响的内在原因．     

Cadmium (II) pyrrolidine dithiocarbamate complex as single source precursor for the preparation of CdS nanocrystals by microwave irradiation and conventional heating process

The complex of cadmium with pyrrolidine dithiocarbamate Cd(pdtc)₂ has been used as single source precursor for the synthesis of CdS nanoparticles. The formation of CdS nanostructures was achieved by thermal decomposition of the complex under microwave irradiation and conventional heating in presence of hexadecylamine. The CdS nanoparticles with disordered close-packed structure were obtained under microwave irradiation, whereas wurtzite hexagonal phase CdS nanorods were obtained by conventional heating method (up to 150 °C). Scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and high resolution transmission electron microscopy (HRTEM) studies also were carried out to study the structure and morphology of nanoparticles. The optical property of the CdS nanoparticles was studied by UV-visible and fluorescence emission spectral studies. Fluorescence measurements on the CdS nanoparticles show a strong emission spectrum with two sub bands that are attributed to band-edge and surface-defect emissions. The reduction of a suitable cadmium metal complex is considered to be one of the single pot methods to generate CdS semiconductor nanoparticles with different shapes and high yield.     

Influence of low-energy Argon ions on thermal and surface properties of polycarbonate films

Low-energy Argon ions from electron cyclotron resonance ion source were bombarded on polycarbonate films. The interaction of ions with the surface of the material was studied by using X-ray diffraction analysis, Fourier transform infrared spectroscopy, thermo-gravimetric analysis and atomic force microscopy. The study reveals that the surface roughness of the films increases with the modification of the surface morphology induced by ion irradiation. Thermal decomposition zone of irradiated samples has extended and hence thermal stability has also improved. Changes in the structural parameters and functional groups were observed after irradiation. These ion-induced changes and their significance were discussed in this paper.     

Thermal release of trapped deuterium from silica injected by 80-keV D+ ion implantation and RF D2 plasma

When silica is irradiated by 80-keV D⁺ ions or RF plasma of D₂ gas, deuterium is trapped in the silica forming Si-OD bonds. The deuterium, trapped as OD bonds, is desorbed from the silica upon heating to form some release products. The thermal detrapping process corresponds to decrease of OD bonds and was studied by measurement of infrared Fourier transform spectroscopy (FTIR). The release products HDO, D₂O, HD, and D₂ were measured by quadrupole mass spectroscopy (QMS). The detrapping and release processes of trapped deuterium were studied by simultaneous measurement of FTIR and QMS. Since the release spectra of HDO, D₂O, HD, and/or D₂ correspond to the decrease spectra of OD bonds, these release products are formed by thermal decomposition of OD bonds. The formation of water (HDO, D₂O) and hydrogen (HD, D₂) depends upon concentration of pre-existing OH bonds and deuterium injection methods (80-keV D⁺ implantation or RF D₂ plasma irradiation).