Use of high temperature X-ray diffraction and pair distribution function for the study of carbonation characteristics of Barium Titanate at nanoscale

Barium titanate (BT) is extensively used in electronic industries for its high dielectric constant. However, the dielectric properties of BT significantly change due to carbonation at nanoscale. Commercially available tetragonal BT powder was milled to study the local atomic distribution and phase transformation behaviour with temperature. Nano BT powder was prepared by the high energy ball milling (90 h) from its bulk counterpart. It was carbonated when it was exposed to open atmosphere. The milled BT sample was characterised by high temperature X-ray diffraction (HT-XRD), pair distribution function (PDF) and transmission electron microscope (TEM). Local atomic distribution was obtained from PDF analysis. The peak due to C-O and Ba-C pair distance were observed from PDF for 90 h milled carbonated BT. TEM analysis revealed that particle diameter was in the range of 15-50 nm. How the phase of nano BT ceramics transformed with temperature was strudied. It was observed that orthorhombic BT transformed into tetragonal and cubic phase via the monoclinic phase during heating at 900 degrees C. Coexistence of multi phases of BT was also observed from HT-XRD. BaCO3 disappeared at high temperature

Ambient formation of high pressure Ag2Si2O5 and non-stoichiometric Ag0.3Al0.7 alloy under confinement

We report results of Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive Analysis of X-rays (EDAX), X-ray Photoelectron Spectroscopy (XPS), X-ray Reflectivity (XRR), and X-ray Diffraction (XRD) and residual stress measurement studies of Ag-silica composite films on Al(001) co-deposited from precursors and spin-coated at different frequencies under ambient conditions. FESEM and EDAX show Ag nanoparticle formation, and XRD, XPS, and XRR show Ag0.3Al0.7 alloy and Ag-rich silicate Ag2Si2O5 formation in all samples. The alloy is non-stoichiometric and non-equilibrium, while the silicate forms at high oxygen pressure. XRR shows the presence of three layers, nanoparticles on top, silicate in the middle, and alloy at the bottom, on an Ag-doped Al substrate. Film thickness decreases exponentially with frequency. Individual layers increase in crystal domain size with a frequency of 3000 rpm when the silicate layer thins below unit cell thickness and the growth has a two-dimensional preference. Our results suggest total confinement by film thinning and local confinement from the Ag nanolayer. Residual stress measurements on the films deposited at 500 and 5000 rpms show a gradual increase in the tensile stress. The increase in spinning frequency reveals the formation of high pressure ambience

Laboratory X-ray diffractometer for PDF experiments using Ag radiation

The conventional crystallographic structure solution by X-ray Diffraction technique using Rietveld method prove its great potential for determination of the average structure of the materials for long range periodicity. Experimentally, the structural information of long range periodic atomic ordering of material is reflected in the Bragg’s peaks while local or short rangestructure is reflected in the diffuse peaks. In order to obtain structural information about both average and local atomic structures, need a technique that will consider both Braggs peaks as well as diffuse peaks. Therefore, Total Scattering Atomic Pair Distribution Function (PDF) technique based on Debye Scattering function will be the only possible solution. Atpresent synchrotron and neutron sources are the choice for PDF analysis for short range structure study. But there is a need for routine analysis of such type of samples in a conventional laboratory XRD system to get the quick feedback about the short range structure. PDF analysis can be performed in a Laboratory X-ray diffractometer using Ag radiation (λ =0.5608 Å) to obtain maximum Q value i.e. 22 Å-1. The present work will report PDF based methodology in a laboratory XRD system to extract structural information about nanostructured and disordered materials over short and long range for structural characterization of crystalline and amorphous materials.Present work will report how this PDF technique used to unravel the structure of disordered materials and nanomaterials like amorphous silica, Ni, nano Ba-based Perovskite, etc for better understanding the materials at nano level. Structural information as obtained by the PDF analysis will help to control the performance of the disordered materials for tailoring thematerials at nano scale. This method may be applicable to the characterization of the nanoscale crystalline and amorphous materials based on PDF analysis in Laboratory XRD system using Ag Radiation. This proposed experimental technique will help to quick feedback about local or disordered structure based on PDF using Ag radiation in a laboratory XRD system