Volume 28(1) - Winter 2012

Lithium ion battery (LIB) has been successfully applied to portable electronics for the last decade.  Recently, application of LIB in the field of energy vehicles and stationary storage systems has attracted considerable attention, in order to efficiently utilize renewable energies such as solar and wind energies. As higher energy capacity and power, long-term stability, safety, and lower costs are required, further development and studies are accelerated around the globe. To attain this goal, extensive research about the materials and the configurations of the battery is being carried out. In addition, characterization techniques are strongly required because it is essential to understand the fundamental behavior of the material in the electrochemical reaction, the mechanism of cell deterioration, the interphase phenomena of the electrode and electrolyte, and many indeterminate ideas not yet well understood.

The materials used in the manufacture of lithium-ion batteries include positive electrode materials, negative electrode materials, electrolytes, separators, binders (for positive and negative electrodes), and cladding materials (for battery housings). Research and development on these materials is active and ongoing.

This paper describes recent expectations for X-ray diffractometers in research and development activities that seek to improve the performance of such materials.  It also introduces measurement methods that respond to those expectations.

The various XRD techniques as the characterization tools for thin film samples have been presented in this series of “X-ray thin-film measurement technique” lecture course. There has heretofore been remarkable progress with detectors equipped with XRD apparatus.  In this lecture, some explanation of the features and functions of 1-dimensional (1D)/2-dimensional (2D) detectors should be presented before summarizing this technical lecture course.

All substances around us consist of atoms. The types of atoms and their three-dimensional arrangement define the structure of materials, therefore the nature of materials. Since the properties and functions of materials relate directly to its structure, there exist extensive researches for various materials such as semiconductor, electronic, food, pharmaceutical, or life science related materials.

However, we can’t recognize the structure of materials at the atomic level because of the limited resolution mainly due to the wavelength, as long as we see objects with our eyes by using visible light. For example, we neither can distinguish a grain of table salt from that of sugar by their atomic level structures, nor can have a clear view of the turtle shell-shaped 6-membered rings (benzene rings) by just staring at the medicine for colds.

Recently, elucidation of molecular structures is becoming more common owing to the developments of various measurement techniques. Nuclear magnetic resonance (NMR), mass spectrometry (MS), and infrared spectroscopy (IR) are the typical examples.  However, these spectroscopic techniques derive just a list of partial structures, and it is sometimes difficult to deduce the three-dimensional structure of a whole molecule. On the other hand, it is the molecular structure itself that is derived from the single crystal X-ray analysis (SCXRD). The single crystal analysis provides a unanimous conclusion that sometimes puts an end to arguments over molecular or crystal structures.

However, it is the fact that X-ray crystallography tends to be averted despite its efficiencies because it gives an impression to be difficult method requiring special knowledge. Through this series of articles, we would like to deliver an introductory course to the single crystal X-ray analysis to those who are not familiar with this technique. The course includes what X-ray crystallography is, what X-ray crystallography reveals, and how to solve the problems you will encounter in the future.
 

Although thermal analysis has wide range of applications, to understand thermophysical and chemical changes at a macro-molecular level, it is necessary to perform complex measurements, such as hyphenated methodology combined with other spectroscopic methods to obtain specific micro-molecular information on reaction products. An example of a complex measurement is the thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS), which is a simultaneous measurement technique composed of thermogravimetry-differential thermal analysis (TG-DTA) combined with mass spectrometry (MS) through an interface system. This process has garnered attention as a major thermoanalytical technique. It is suitable for the qualitative analysis of the different gases evolved in response to heating a sample in the TG-DTA process.

This article aims to propose a novel thermoanalytical method that integrates a “skimmer-type interface” and a “photoionization method” in order to overcome the serious disadvantages of the conventional TG-DTA-MS.  A simultaneous thermogravimetry-differential thermal analysis and photoionization mass spectrometry (TGDTA- PIMS) system equipped with a unique skimmertype interface has been thus successfully developed.

The principles and the instrumental composition of the TG-DTA-PIMS are described in detail and compared with those of the conventional TG-DTA-MS. To demonstrate the effectiveness of the technique, the results of its application to the evolved gas analysis of typical polymeric materials are presented.
 

Total reflection X-ray fluorescence (TXRF) spectrometry is widely used in semiconductor manufacturing processes for nondestructive analyses of metallic contamination on wafer surfaces.  Sensitivity requirements for such devices have increased in recent years. Currently, metallic contamination in advanced device manufacturing processes is controlled to 10⁸ atoms/cm². In a conflicting trend, the growing diversification of semiconductor devices has generated demand for low-cost equipment with advanced functionality rather than sensitivity. The TXRF 3800e is a low-cost, total reflection X-ray fluorescence spectrometer with advanced functions that meets these demands.

PDXL is a one-stop powder diffraction analysis software suite. The advanced engine and userfriendly GUI have been satisfying both experienced and novice users since PDXL was released in 2007.

PDXL provides various analysis tools such as automatic phase identification, quantitative analysis, crystallite-size analysis, lattice constants refinement, Rietveld analysis, ab initio structure determination, etc.

In May 2011, Rigaku released a new version “PDXL 2” with several excellent new features, which are introduced in the following sections.