Thermal analysis is widely used in the pharmaceutical industry to measure properties such as polymorphism, excipient compatibility, purity, melting points and humidity studies
Since there is a strong relation between the material characteristics and the crystal orientation of metals and many other industrial materials, quantitative analyses of crystallites orientation and their distributions are of great importance. Pole figure measurements are a common method to quantitatively analyze orientation. In this Application Byte, we used the Orientation Distribution Function (ODF) to evaluate the crystallites orientation of a Cu wiring film from a pole figure measurement.
Quantitative analysis by powder X-ray diffraction has long been carried out using calibration curves, a
technique that requires preparing samples whose components are quantified, using pure or standard
substances to obtain calibration curves. In recent years, quantitative analysis without calibration curves has
become possible by calculating quantitative values from crystal structures. However, these methods require
the crystal structures of the materials, limiting the applicable substances. With the Direct Derivation method
introduced here, the quantitative weight fractions of individual crystalline phases can be derived from sets of
integrated intensities collected in a wide 2 range, together with chemical composition data.
The Oido tunnel tombs in Wakuyacho, Miyagi (Japan) are tumuli that have been constructed between the late 7th century and the early 8th century. During scientific investigations between 1962 and 1964, a glass bead with a spotted pattern (concentric circles) rare to Japan was excavated, which is believed to be originated in South Asia or Southeast Asia. By evaluating the colored portion of the glass bead using the SmartLab Automated Multipurpose X-ray Diffractometer, it was possible to determine its chemical composition and provide a scientific basis for assumptions on the fabrication technique and a reevaluation of its origin. The research was conducted by the Nara National Research Institute for Cultural Properties in 2013, and presented at the 31st Congress of the Japan Society for Scientific Studies on Cultural Properties in 2014.
Thin films formed on substrates show various crystal phase and orientations depending on the materials and
manufacturing method. Therefore, phase identification is sometimes difficult by ordinary X-ray diffraction
(XRD) measurement. The diffraction image using a two-dimensional (2D) detector reveals the lattice constant
and the orientation for each crystal phase readily because the diffraction intensity distribution in the 2θ
direction and the distribution of the crystal orientation in the χ direction are observed simultaneously.
In the tableting process for pharmaceuticals, it sometimes happens that the active pharmaceutical ingredient reacts with materials used as excipients, such as sugar or starch, and dehydration reactions, polymorph transitions and other processes may occur due to the pressure during tableting. In recent years, a need has arisen to check, in the shortest possible time, whether or not the active pharmaceutical ingredient maintains its original crystal system, and whether or not there are polymorph impurities. Furthermore, this must be done in the tableting process, while maintaining the tablet form. Therefore, we used a powder X-ray diffractometer to non-destructively measure the state of tablets in their original form, and evaluate the presence of the contained active pharmaceutical ingredient and polymorph impurities. By using a transmission-type parallel beam optical system, it is possible to obtain an accurate diffraction profile which does not depend on the sample form, and acquire information not only from the outside, but also from the inside of tablets. As a result of measurement, it was found that if polymorph impurities of the active pharmaceutical ingredient are about 1%, then their presence in the tablets could be confirmed in a measurement time of less than 10 minutes.
Carbide tools used for cutting are provided with various types of coatings to improve durability. Previously, evaluation of the coating layer has been done using X-ray diffraction, but some users want to achieve rapid and simultaneous evaluation of factors such as site-dependent differences in composition, crystallinity and orientation. These evaluations can be easily done by employing the optical element and detector used in this report.
Controlling the state of the charge-discharge process is believed to be crucial for extending the life of lithium ion batteries. Therefore, it is not enough to simply observe the electrode structure in the 100% charged and discharged states, and there is a need to carry out in-situ observation of the relationship between depth of charge, depth of discharge and electrode structure. However, if materials are removed once from sealed batteries, the materials will react with the atmosphere, and the charge-discharge state will change due to peeling of electrodes. Thus there is a risk of the material changing into another structure, irrespective of the charge-discharge situation. As a result, with previous methods, it was difficult to observe changes in materials accompanying charging-discharging via an X-ray diffraction measurement. However, with batteries made using lithium ion battery cells for evaluation and testing, X-ray diffraction can be performed simultaneously with charge-discharge testing. Thus it is possible to carry out evaluation by directly relating changes in the state of samples to charge-discharge characteristics, without performing any additional work on the materials subjected to charge-discharge testing, such as opening seals or peeling electrodes.
To capture the moment when materials change, such as during melting, solidification or crystal phase change,
by in-situ X-ray diffraction measurement, the acquisition time of the X-ray diffraction images at each
temperature needs to be as short as possible. 0D and 1D detectors take time to scan the detector and
prepare for operation. Conventional 2D detectors also have a problem in that the X-ray shutter needs to be
opened and closed between counting and reading the data. The HyPix-3000 hybrid pixel array
multi-dimensional detector in 2D mode can acquire X-ray diffraction images without scanning the detector.
The HyPix-3000 has two counters inside. Switching between them allows measurement without dead time.
These features enable shutterless measurement of 2D X-ray diffraction images, which makes it possible to
observe rapid changes in crystalline state.
Reciprocal space mapping (RSM) is an XRD technique used to evaluate lattice spacing and crystal orientation
distribution independently from each other, applied to the analysis of thin film samples such as epitaxial films.
Since a reciprocal space map requires multiple scans with various combinations of the scattering angle (2θ)
and the incident angle with respect to the sample (ω), it can take a relatively long time to collect the necessary
data in general. Combination of the 1D exposure mode of a 2D detector and high-speed scanning by the ω
axis enables data collection in a very short time, from several tens of seconds to several minutes,