Depth profiling spatial resolution

In summary, CL can provide contactless and nondestructive analysis of a wide range of electronic properties of a variety of luminescent materials. Spatial resolution of less than 1 pm in the CL-SEM mode and detection limits of impurity concentrations down to 10 at/cm can be attained. CL depth profiling can be performed by varying the range of electron penetration that depends on the electron-beam energy the excitation depth can be varied from about 10 nm to several pm for electron-beam energies ranging between about 1 keV and 40 keV. 

Like XPS, the application of AES has been very widespread, particularly in the earlier years of its existence more recently, the technique has been applied increasingly to those problem areas that need the high spatial resolution that AES can provide and XPS, currently, cannot. Because data acquisition in AES is faster than in XPS, it is also employed widely in routine quality control by surface analysis of random samples from production lines of for example, integrated circuits. In the semiconductor industry, in particular, SIMS is a competing method. Note that AES and XPS on the one hand and SIMS/SNMS on the other, both in depth-profiling mode, are complementary, the former gaining signal from the sputter-modified surface and the latter from the flux of sputtered particles. 

FTIR also has several disadvantages. For example, depth profiling is not possible in RAIR. In ATR, surfaee sensitivity is limited to approximately the wavelength of infrared radiation or about one micrometer (see below). The spatial resolution of eonventional infrared teehniques is limited by diffraetion effeets and is only approximately a few tens of micrometers. 

However, the spatial resolution of AES is mueh greater than that of XPS and ean approaeh approximately 25 nm. This makes AES a powerful technique for constructing high-resolution maps showing the distribution of chemical species across a surface. Because of the small analysis area, it is an easy matter to combine AES with inert gas sputtering to construct depth profiles showing the distribution of chemical species as a function of distance away from the surface and into the bulk of the solid. Quantitative analysis can be done using sensitivity factors and an equation similar to Eq. 17. 

The Physical Electronics 680 Nanoprobe employs a field emission electron gun, and this results in a spatial resolution of less than lOnm. Ion bombardment for depth profiling is available in the SAM, and both the electron beam and the ion beam are computer controlled so that depth profiles can be run automatically, and maps and line scan of Auger electron distributions can be generated. 

NRA is a powerful method of obtaining concentration versus depth profiles of labelled polymer chains in films up to several microns thick with a spatial resolution of down to a few nanometres. This involves the detection of gamma rays produced by irradiation by energetic ions to induce a resonant nuclear reaction at various depths in the sample. In order to avoid permanent radioactivity in the specimen, the energy of the projectile is maintained at a relatively low value. Due to the large coulomb barrier around heavy nuclei, only light nuclei may be easily identified (atomic mass < 30). 

Depth profiles of matrix elements on Mn- and Co-perovskite layers of fuel cathodes have been measured by LA-ICP-MS in comparison to other well established surface analytical techniques (e.g., SEM-EDX).118 On perovskite layers at a spatial resolution of 100p.m a depth resolution of 100-200 nm was obtained by LA-ICP-MS. The advantages of LA-ICP-MS in comparison to other surface analytical techniques (such as XPS, AES, SIMS, SNMS, GD-OES, GDMS and SEM-EDX) are the speed, flexibility and relatively low detection limits with an easy calibration procedure. In addition, thick oxide layers can be analyzed directly and no charging effects are observed in the analysis of non-conducting thick layers. 

The development of surface analytical techniques such as LA-ICP-MS, GDMS and SIMS focuses on improvements to sensitivity and detection limits in order to obtain precise and accurate analytical data. With respect to surface analytical investigations, an improvement of spatial and depth resolution is required, e.g., by the establishment of a near field effect or the apphcation of fs lasers in LA-ICP-MS. There is a need for the improvement of analytical techniques in the (j,m and nm range, in depth profiling analysis and especially in imaging mass spectrometry techniques to perform surface analyses faster and provide more accurate data on different materials to produce quantitative 3D elemental, isotopic and molecular distribution patterns of increased areas of interest with high spatial and depth resolution over an acceptable analysis time. 

PIGE is very sensitive (the limit of detection can be as low as 1 ppm) and non-destructive. It allows analysis of bulk F, F-distribution within one sample on cross-sections or depth profiles using resonant nuclear reaction analysis (RNRA) [35]. The spatial resolution, even using a beam of some micrometres size or RNRA, is however insufficient to detect F on individual bone crystals. The RNRA method is reviewed in detail in the chapter of Dobeli et al. [6] in this volume. 

SIMS has become one of the most important tools for the characterization of experimental products because of its minimal sample requirements, high spatial resolution, excellent sensitivity, and unsurpassed ability for depth-profile measurements. Most of the experimental work can be split into two different areas. The first consists of studies examining diffusion rates of different elements in minerals or melts under a variety of pressure, temperature, and fluid conditions, typically by using an isotopically enriched tracer. These analyses are done either by cutting a surface parallel to the diffusion direction and taking a traverse of spot analyses (for conditions in which profiles in the tens to hundreds of micrometers are expected) or by depth-profiling in from the mineral surface to depths of as much as 5-10 micrometers. In the latter mode, depth resolution on the tens of nanometer scale is possible (see Chapter 4). The second area is focused on determining partition coefficients for trace elements between different minerals and fluids/melts at specific temperatures, pressures, and fluid conditions, to provide the data needed to interpret trace element contents measured in natural minerals. This type of analysis typically involves spot analysis of mineral run products. 

Secondary ion mass spectrometry is based on surface bombardment by argon ions in UHV, followed by mass spectrometry of the charged species which are sputtered from the sample s surface. It provides specific information on surface species, high spatial resolution and depth profiling [64], The SIMS requires an... 

Fig. 31. Plot of interfacial width w vs D for a blend of olefinic copolymers d75/h66 (cf.text) at T0=356 K, extracted from nuclear reaction depth profiling experiments, based on the reaction 3He+2H 4He+1H+18.35 MeV and backward angle detection of 1H. Note that the spatial resolution is optimal near the air surface (4 nm) but quickly deteriorates for large distances from the air surface. Therefore, the error bar on w/2 increases strongly with increasing D. Full and dotted curves represent the approximate asymptotic formula w2 = Wq + D / 4 (a factor 7tco/(l+co/2) in Eq. (127) being approximated as unity), choosing w0= b> and b=l 1 8 nm or b=10.6 nm, respectively. From Kerle et al. [84]...

Comparative studies of neodymium measurements in UOj fuel for the future application of local burn up calculations have been carried out by the SIMS analysis of a Nd implanted UOj single crystal. Samples for a round robin test were produced by the implantation of " Nd (5 x 10 ° at cm , 400 keV) in a UOj single crystal. Different depth profiles of the Nd "/ U+ ratio and especially the NdO /Nd, UO+/U+ and U02 /U+ ratios obtained by SIMS are not constant over time and indicate evidence of some fluctuations during the analysis. SIMS plays a dominant role for particle analysis, but also LA-ICP-MS with lower spatial resolution can be applied to identify anomalies in the isotopic composition of radionuclides. 

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