Energy dispersive spectroscopy characterization

Catalysts were characterized using SEM (Hitachi S-4800, operated at 15 keV for secondary electron imaging and energy dispersive spectroscopy (EDS)), XRD (Bruker D4 Endeavor with Cu K radiation operated at 40 kV and 40 mA), TEM (Tecnai S-20, operated at 200 keV) and temperature-programmed reduction (TPR). Table 1 lists BET surface area for the selected catalysts. 

Although a number of secondary minerals have been predicted to form in weathered CCB materials, few have been positively identified by physical characterization methods. Secondary phases in CCB materials may be difficult or impossible to characterize due to their low abundance and small particle size. Conventional mineral identification methods such as X-ray diffraction (XRD) analysis fail to identify secondary phases that are less than 1-5% by weight of the CCB or are X-ray amorphous. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM), coupled with energy dispersive spectroscopy (EDS), can often identify phases not seen by XRD. Additional analytical methods used to characterize trace secondary phases include infrared (IR) spectroscopy, electron microprobe (EMP) analysis, differential thermal analysis (DTA), and various synchrotron radiation techniques (e.g., micro-XRD, X-ray absorption near-eidge spectroscopy [XANES], X-ray absorption fine-structure [XAFSJ). 

This chapter summarizes results obtained during the past 5 years, on the design, preparation and study of titanium and vanadium compounds as candidate precursors to TiC, TiN, VC, and VN. The study of the precursor molecules was conducted through several steps. After their synthesis, thermoanalytical studies (TG-DTA), coupled to simultaneous mass spectroscopic (MS) analysis of the decomposition gases, were carried out to determine their suitability as precursors. CVD experiments were then conducted and were followed by characterization of the deposits by scanning electron microscopy (SEM) energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and electron microprobe analysis with wavelength dispersion spectroscopy (EPMA-WDS). 

A novel chemical functionalization method for MWCNTs through an oxidation and silylation process was reported in 2002. Purified and oxidatively functionalized MWCNTs were reacted with 3-mercaptopropyltrimethoxysilane, the CNT surface being joined to the organosilane moieties through OH groups [143], Similarly, MWCNTs were functionalized by KMn04 oxidation under PTC catalysis and subsequent reaction with the hydrolysis product of 3-methacryloxypropyltri-methoxysilane (3-MPTS) (Scheme 1.13). The O-silyl-functionalized MWCNTs were characterized by FT-IR spectroscopy and energy-dispersive spectroscopy... 

Particles of Raney copper, modified by redox deposition of ruthenium, platinum, or gold were characterized by energy dispersive spectroscopy. Ruthenium is deposited preferentially on the rims of the copper particles while low Miller-index planes are totally free of deposited ruthenium atoms. For platinum or gold the deposition can occur over the whole copper surface [11]. 

The toxicity of the mineral is such that quantitative characterization of erionite is extremely important. Samples should be characterized by using one or more of the following techniques (1) powder X-ray diffraction, (2) electron probe microanalysis or inductively coupled plasma-mass spectroscopy, (3) scanning electron microscopy equipped with wavelength dispersive spectroscopy (WDS) and/or energy dispersive spectroscopy (EDS), (4) transmission electron microscopy equipped with WDS and/or EDS and selected area electron diffraction, and (5) similar or better analytical techniques. 

Highly cubic ordered cobalt oxides have been successfully synthesized from KlT-6 by an accurately controlled incipient wetness approach. The adding volume of cobalt nitrate and absolute ethanol were determined by the pore volume of KIT-6, and the synthesis procedure is effective and economical. Furthermore, the obtained mesoporous cobalt oxides have better mesostructure comparing with those of former reports. The X-ray diffraction, N2 sorption isotherms, transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDS) and Fourier-transform infrared spectroscopy were used to characterize the as-synthesized mesoporous cohalt oxides. 

Synthesized powders were calcined and characterized by standard techniques of thermogravimetric analysis, BET specific surface area measurements, and particle size determination by sedigraphy, as well as X-ray diffraction, and scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) for microchemical analyses. To... 

This outline of the principal characterization techniques for nanocomposite materials is far from being complete. Advances in Raman spectroscopy, energy dispersive spectroscopy, infrared spectroscopy, and many other techniques are of considerable importance as well. In fact, the success that nanos-tructured materials are having in the last few years is strictly related to the advanced characterization techniques that are available today. 

Alternatively, hydrophilic multi-hydroxyl poly(GMA-OH)-grafted MWCNTs could be converted into multicarboxyl polymer-functionalized CNTs by reaction with succinic anhydride and then used as templates to efficiently sequestrate metal ions such as Ag", Co ", Ni , Au , La and (Scheme 5.3), generating MWCNT-polymer/metal hybrid nanocomposites, nanowires or necklace-like nanostructures, depending on the grafted polymer content and the nature of the captured metals. The combination of SEM, TEM and energy dispersive spectroscopy (EDS) characterizations demonstrated the structure and elements of the hybrid nano-objects. 

Common techniques for the characterization of the electrocatalysts include High Resolution Electron Microscopy (HRTEM), Extended X-ray Absorption Fine Stracture Spectroscopy (EXAFS), Energy Dispersive Spectroscopy (EDS), Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES), Near Edge X-ray Absorption Spectroscopy (XANES), X-Ray Powder Diffraction (XRPD), Infrared and Raman Spectroscopy (IR, RS). 

SEM is probably the optimal method for characterizing the particle morphology— shape, size, and porosity. With the addition of energy-dispersive spectroscopy (EDS) or wavelength-dispersive spectroscopy (WDS), the elemental composition of the particle can also be obtained in the SEM. The whole stub can be transferred to a SIMS chamber or LA-ICPMS cell and the coordinates of the particles, obtained from the SEM, can be used for direct measurement of the isotopic composition or, as mentioned earlier, individual particles can be manipulated and transferred. 

Techniques used to characterize these nanocomposites included transmission electron microscopy (TEM) using a Philips CM20T TEM operating at 200 kV and equipped for selected area electron diffraction and energy dispersive spectroscopy... 

---