Electron-induced X-ray emission

Electron Microprobe A.na.Iysis, Electron microprobe analysis (ema) is a technique based on x-ray fluorescence from atoms in the near-surface region of a material stimulated by a focused beam of high energy electrons (7—9,30). Essentially, this method is based on electron-induced x-ray emission as opposed to x-ray-induced x-ray emission, which forms the basis of conventional x-ray fluorescence (xrf) spectroscopy (31). The microprobe form of this x-ray fluorescence spectroscopy was first developed by Castaing in 1951 (32), and today is a mature technique. Primary beam electrons with energies of 10—30 keV are used and sample the material to a depth on the order of 1 pm. X-rays from all elements with the exception of H, He, and Li can be detected. 

The X-ray emission process followii the excitation is the same in all three cases, as it is also for the electron-induced X-ray emission methods (EDS and EMPA) described in Chapter 3. The electron core hole produced by the excitation is filled by an electron falling from a shallower level, the excess energy produced being released as an emitted X ray with a wavelength characteristic of the atomic energy levels involved. Thus elemental identification is provided and quantification can be obtained from intensities. The practical differences between the techniques come from the consequences of using the different excitation sources. 

Taftp, J. (1982) The cation-atom distribution in a (Cr,Fe,Al,Mg)304 spinel as revealed from the channeling effect in electron-induced X-ray emission. J. Appl. Crystallogr., 15, 378-81. 

X-ray fluorescence analysis electron induced X-ray emission elements as from atomic number 12 and their compounds few monolyers 100-400 + A yes yes depending on the atomic number of the element [49-52] [73]... 

Analytical electron microscopy (AEM) permits the determination of the elemental composition of a solid catalyst at the microscopic level by energy-dispersive detection of the electron-induced X-ray emission (EDX). Energy dispersive spectroscopy (EDS) is sensitive for elements with atomic numbers Z > 11. For lighter elements (Z < 11), electron energy loss spectroscopy (EELS) is applied. An example is shown in Figure 7 (bottom), which exhibits the elemental composition by EDX of two individual Pt/Rh particles on a carbon film. This analysis clearly demonstrates the heterogeneous composition of the alloy particles. 

Neutron Activation Analysis X-Ray Fluorescence Particle-Induced X-Ray Emission Particle-Induced Nuclear Reaction Analysis Rutherford Backscattering Spectrometry Spark Source Mass Spectrometry Glow Discharge Mass Spectrometry Electron Microprobe Analysis Laser Microprobe Analysis Secondary Ion Mass Analysis Micro-PIXE... 

There are two principal sources of reliable partitioning data for any trace element glassy volcanic rocks and high temperature experiments. For the reasons outlined above, both sources rely on analytical techniques with high spatial resolution. Typically these are microbeam techniques, such as electron-microprobe (EMPA), laser ablation ICP-MS, ion-microprobe secondary ion mass spectrometry (SIMS) or proton-induced X-ray emission (PIXE). 

Particle-induced X-ray emission (PIXE) in which electrons are ionised, and elemental specific X-rays are generated by the incident ion beam. 

Ion beam spectrochemical analysis Auger emission spectroscopy Scanning electron microscopy (SEM) Electron microprobe (EMPA) Particle-induced X-ray emission spectroscopy (PIXE)... 

There are now several different types of machines that are all capable of microanalysis. All have advantages and disadvantages, but the choice of which to use is often governed by expense and availability to a particular institution. Electron probe microanalysis is by far the most popular, but here particle-induced X-ray emission (PIXE), the laser microprobe mass analyzer (LAMMA), electron energy loss spectroscopy (EELS), and secondary ion mass spectrometry (SIMS) are also considered. 

Three analytical techniques which differ in how the primary vacancies are created share the use of such X-rays to identify the elements present. In X-ray fluorescence, the solid sample is irradiated by an X-ray beam (called the primary beam), which interacts with the atoms in the solid to create inner shell vacancies, which then de-excite via the emission of secondary or fluorescent X-rays - hence the name of the technique. The second uses a beam of electrons to create the initial vacancies, giving rise to the family of techniques known collectively as electron microscopy. The third and most recently developed instrumentation uses (usually) a proton beam to cause the initial vacancies, and is known as particle- (or proton-) induced X-ray emission (PIXE). 

This chapter discusses the range of analytical methods which use the properties of X-rays to identify composition. The methods fall into two distinct groups those which study X-rays produced by the atoms to chemically identify the elements present, and X-ray diffraction (XRD), which uses X-rays of known wavelengths to determine the spacing in crystalline structures and therefore identify chemical compounds. The first group includes a variety of methods to identify the elements present, all of which examine the X-rays produced when vacancies in the inner electron shells are filled. These methods vary in how the primary vacancies in the inner electron shell are created. X-ray fluorescence (XRF) uses an X-ray beam to create inner shell vacancies analytical electron microscopy uses electrons, and particle (or proton) induced X-ray emission (PIXE) uses a proton beam. More detailed information on the techniques described here can be found in Ewing (1985, 1997) and Fifield and Kealey (2000). 

Protons can also be used instead of X-rays or electrons to create the initial vacancies in the inner electron shells, giving rise to a method known as proton induced X-ray emission (PIXE). In these instruments a high intensity, highly focused beam of protons is produced by a van de Graaff accelerator,... 

Another important characteristic is that ion beams can produce a variety of the secondary particles/photons such as secondary ions/atoms, electrons, positrons. X-rays, gamma rays, and so on, which enable us to use ion beams as analytical probes. Ion beam analyses are characterized by the respectively detected secondary species, such as secondary ion mass spectrometry (SIMS), sputtered neutral mass spectrometry (SNMS), electron spectroscopy, particle-induced X-ray emission (PIXE), nuclear reaction analyses (NRA), positron emission tomography (PET), and so on. 

Brands proposed a calculation method in the case of segregation A special type of inhomogeneous, particulate objects is the surface analysis by microscopic techniques e.g. analytical electron sj troscopy, laser induced mass spectroscopy or proton-induced X-ray emission. Here the minimum sample size can be translated into the minimum number of specific sample points in the specimen under investigation. 

Particle-induced X-ray emission (PIXE) is an analytical technique based upon observing fluorescent X-rays. As such, it really is not a nuclear technique since it involves an atomic process, X-ray emission. But the atomic electron shell vacancies that are filled when the X-ray is emitted are created using particle-accelerator beams and one uses typical semiconductor radiation detectors, Si (Li) detectors, to detect the X-rays. 

High-resolution compositional measurements are possible through use of a variety of microanalytical methods. Ideally, these should be non-destructive, can be targeted on small areas of sample, and have low minimum detection limits. Electron-probe X-ray microanalysis (EPXMA) and proton-induced X-ray emission (PIXE) techniques have both been used successfully on archaeological sediment thin sections (19, 20). Both techniques yield elemental composition data for a range of elements. EPXMA has the advantage of being nondestructive, whereas PIXE when used on thin-section samples is typically destructive conversely the detection limit for PIXE is lower than EPXMA. 

The use of particles heavier than electrons, and especially proton-induced x-ray emission analysis, was developed under the supervison of Professor Sven Johansson at Lund University, Sweden, during the 1970s.9 Generally referred to as PIXE (particle- or proton-induced x-ray emission) analysis, it has proven to be a sensitive trace element technique. The initial response among medical researchers was a cautious one, most likely due to the fact that the problems of specimen preparation initially were... 

Malmquist, K.G. etal., Proton-induced x-ray emission analysis — a new tool in quantitative dermatology, Scanning Electron Microsc, 4, 1815, 1983. 

Forslind, B. etal., Elemental analysis on freeze dried sections of human skin studies by electron microprobe and particle induced x-ray emission analysis, Scanning Electron Microsc., 2, 755, 1984. 

Pt-Re Coimpregnated on A1203./ - / sulfided Proton induced X-ray emission, Rutherford backscattering, electron microscopy. 

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