Energy Dispersive X-Ray Spectroscopy (2)

Elemental Mapping - Characteristic x-ray intensity is measured relative to lateral position on the sample. Variations in x-ray intensity at any characteristic energy value indicate the relative concentration for the applicable element across the surface. One or more maps are recorded simultaneously using image brightness intensity as a function of the local relative concentration of the element(s) present. About 1 µm lateral resolution is possible.

Line Profile Analysis - The SEM electron beam is scanned along a preselected line across the sample while x-rays are detected for discrete positions along the line. Analysis of the x-ray energy spectrum at each position provides plots of the relative elemental concentration for each element versus position along the line.

TYPICAL APPLICATIONS

• Foreign material analysis
• Corrosion evaluation
• Coating composition analysis
• Rapid material alloy identification
• Small component material analysis
• Phase identification and distribution

SAMPLE REQUIREMENTS

Samples up to 8 in. (200 mm) in diameter can be readily analyzed in the SEM. Larger samples, up to approximately 12 in. (300 mm) in diameter, can be loaded with limited stage movement. A maximum sample height of approximately 2 in. (50 mm) can be accommodated. Samples must also be compatible with a moderate vacuum atmosphere (pressures of 2 Torr or less).

Energy Dispersive X-Ray Spectroscopy (1)

DESCRIPTION OF TECHNIQUE

Energy Dispersive X-Ray Spectroscopy (EDS or EDX) is a chemical microanalysis technique used in conjunction with scanning electron microscopy (SEM). (See Handbook section on SEM.)The EDS technique detects x-rays emitted from the sample during bombardment by an electron beam to characterize the elemental composition of the analyzed volume. Features or phases as small as 1 µm or less can be analyzed.

When the sample is bombarded by the SEM's electron beam, electrons are ejected from the atoms comprising the sample's surface. The resulting electron vacancies are filled by electrons from a higher state, and an x-ray is emitted to balance the energy difference between the two electrons' states. The x-ray energy is characteristic of the element from which it was emitted.

The EDS x-ray detector measures the relative abundance of emitted x-rays versus their energy. The detector is typically a lithium-drifted silicon, solid-state device. When an incident x-ray strikes the detector, it creates a charge pulse that is proportional to the energy of the x-ray. The charge pulse is converted to a voltage pulse (which remains proportional to the xray energy) by a charge-sensitive preamplifier. The signal is then sent to a multichannel analyzer where the pulses are sorted by voltage. The energy, as determined from the voltage measurement, for each incident x-ray is sent to a computer for display and further data evaluation. The spectrum of x-ray energy versus counts is evaluated to determine the elemental composition of the sampled volume.

ANALYTICAL INFORMATION

Qualitative Analysis - The sample x-ray energy values from the EDS spectrum are compared with known characteristic x-ray energy values to determine the presence of an element in the sample. Elements with atomic numbers ranging from that of beryllium to uranium can be detected. The minimum detection limits vary from approximately 0.1 to a few atom percent, depending on the element and the sample matrix.

Quantitative Analysis - Quantitative results can be obtained from the relative x-ray counts at the characteristic energy levels for the sample constituents. Semi-quantitative results are readily available without standards by using mathematical corrections based on the analysis parameters and the sample composition. The accuracy of standardless analysis depends on the sample composition. Greater accuracy is obtained using known standards with similar structure and composition to that of the unknown sample.

Auger Electron Spectroscopy Part 2

ANALYTICAL INFORMATION

Survey Scan - The position of the peaks in the AES spectrum obtained in a survey scan identifies the elemental composition of the uppermost 20 Å of the analyzed surface.

Multiplex Scan - A higher resolution analysis of the Auger spectrum in the region around a characteristic peak is used for determination of the atomic concentration of the elements identified in the survey scans and, in some cases, chemical state information.

Quantitation - The AES analysis results can be quantified without standards by using the area under the peaks in the AES spectrum and corrections based on elemental sensitivity factors.

Mapping and Line Scans - These are imaging techniques that measure the lateral distribution of elements on the surface. The electron beam is scanned across the sample surface, either along a fixed line (line scan) or across a given area (mapping) while the AES signal is analyzed for specific energy channels. The AES signal intensity is a function of the relative concentration of the element(s) corresponding to the selected energy channel(s). Spatial resolution is approximately 0.3 µm.

Depth Profile - Material is removed from the surface by sputtering with an energetic ion beam concurrent with successive AES analyses. This process measures the elemental distribution as a function of depth into the sample. Depth resolution of < 100 Å is possible.

TYPICAL APPLICATIONS

Microscopic particle identification
Passive oxide film thickness
Contamination on integrated circuits
Quantitation of light element surface films
Mapping spatial distribution of surface constituents

SAMPLE REQUIREMENTS

Samples should be no larger than approximately 3/4 in. by 1/2 in. (18 mm by 12 mm). Height of samples should not exceed 1/2 in. (12mm). Samples must be conductive or area of interest must be properly grounded. Insulating samples, including thick insulating films (>300 Å), cannot be analyzed. Samples must also be compatible with a high vacuum environment (<1x10^-9 style="margin: 0px auto 10px; display: block; text-align: center; cursor: pointer; width: 318px; height: 198px;" src="https://blogger.googleusercontent.com/img/b/R29vZ2xl/AVvXsEhY76-7x0nKv2x2WrgRFd-TFjAr4YLb1eirX6HecY6SDITaSkVuKkNa_8JkctI96JztvpWLPGX-h_w4xLGCVtxXwcMBEERTfAr4uNmOlfXiicpwoVKOR4KuPrPxnNns0Lilhs_Gg4Yz3G9m/s320/8.JPG" alt="" id="BLOGGER_PHOTO_ID_5322136461000551026" border="0">

Auger Electron Spectroscopy Part 1

DESCRIPTION OF TECHNIQUE

Auger Electron Spectroscopy (AES) provides information about the chemical composition of the outermost material comprising a solid surface or interface. The principal advantages of AES over other surface analysis methods are excellent spatial resolution (< 1 µm), surface sensitivity (~20 Å), and detection of light elements. Detection limits for most elements range from about 0.01 to 0.1 at%.

AES uses a primary electron beam to excite the sample surface. When an inner-shell electron is ejected from a sample atom by the interaction with a primary electron, an electron from an outer shell fills the vacancy. To compensate for the energy change from this transition, an Auger electron or an xray is emitted. For light elements, the probability is greatest for the emission of an Auger electron, which accounts for the light-element sensitivity for this technique.

The energy of the emitted Auger electron is characteristic of the element from which it was emitted. Detection and energy analysis of the emitted Auger electrons produces a spectrum of Auger electron energy versus the relative abundance of electrons. Peaks in the spectrum identify the elemental composition of the sample surface. In some cases, the chemical state of the surface atoms can also be determined from energy shifts and peak shapes.

Auger electrons have relatively low kinetic energy, which limits their escape depth. Any Auger electrons emitted from an interaction below the surface will lose energy through additional scattering reactions along its path to the surface. Auger electrons emitted at a depth greater than about 2 - 3 nm will not have sufficient energy to escape the surface and reach the detector. Thus, the analysis volume for AES extends only to a depth of about 2 nm. Analysis depth is not affected by the energy of the primary electron energy.

The AES instrumentation can include a tungsten filament or field emission electron gun for the primary electron beam. The instruments are equipped for secondary electron imaging (SEM) to facilitate location of selected analysis areas, and micrographs of the sample surface can be obtained. The sample chamber is maintained at ultrahigh vacuum to minimize interception of the Auger electrons by gas molecules between the sample and the detector. Some instruments include special stages for fracturing samples to examine interfaces that have been freshly exposed within the vacuum chamber. A computer is used for acquisition, analysis, and display of the AES data.

Atomic Force Microscopy Part 2

Image Analysis - Since the images are collected in digital format, a wide variety of image manipulations are available for AFM data. Quantitative topographical information, such as lateral spacing, step height, and surface roughness are readily obtained. Images can be presented as two-dimensional or three-dimensional representations in hard copy or as digital image files for electronic transfer and publication.

Nanoindentation - A specialized probe tip is forced into the sample surface to obtain a measure of the material’s mechanical properties in regions as small as a few nanometers. (See the Handbook section on Nanoindentation Hardness Testing.)

TYPICAL APPLICATIONS

• 3-dimensional topography of IC device
• Roughness measurements for chemical mechanical polishing
• Analysis of microscopic phase distribution in polymers
• Mechanical and physical property measurements for thin films
• Imaging magnetic domains on digital storage media
• Imaging of submicron phases in metals
• Defect imaging in IC failure analysis
• Microscopic imaging of fragile biological samples
• Metrology for compact disk stampers

SAMPLE REQUIREMENTS

No sample preparation is typically required. Samples can be imaged in air or liquid. Sample height is limited to about 1.5 inches. Areas up to 8 inches in diameter can be fully traversed without repositioning. Larger samples can be fixtured for imaging within a limited area. Total surface roughness in the image area should not exceed about 6 µm.

Atomic Force Microscopy Part 1

DESCRIPTION OF TECHNIQUE

Atomic Force Microscopy (AFM) is a form of scanning probe microscopy (SPM) where a small probe is scanned across the sample to obtain information about the sample’s surface. The information gathered from the probe’s interaction with the surface can be as simple as physical topography or as diverse as measurements of the material’s physical, magnetic, or chemical properties. These data are collected as the probe is scanned in a raster pattern across the sample to form a map of the measured property relative to the X-Y position. Thus, the AFM microscopic image shows the variation in the measured property, e.g,. height or magnetic domains, over the area imaged.

The AFM probe has a very sharp tip, often less than 100 Å diameter, at the end of a small cantilever beam. The probe is attached to a piezoelectric scanner tube, which scans the probe across a selected area of the sample surface. Interatomic forces between the probe tip and the sample surface cause the cantilever to deflect as the sample’s surface topography (or other properties) changes. A laser light reflected from the back of the cantilever measures the deflection of the cantilever. This information is fed back to a computer, which generates a map of topography and/or other properties of interest. Areas as large as about 100 µm square to less than 100 nm square can be imaged.

ANALYTICAL INFORMATION

Contact Mode AFM - The AFM probe is scanned at a constant force between the probe and the sample surface to obtain a 3D topographical map. When the probe cantilever is deflected by topographical changes, the scanner adjusts the probe position to restore the original cantilever deflection. The scanner position information is used to create a topographical image. Lateral resolution of <1 style="font-weight: bold;">Intermittent Contact (Tapping Mode) AFM - In this mode, the probe cantilever is oscillated at or near its resonant frequency. The oscillating probe tip is then scanned at a height where it barely touches or “taps” the sample surface. The system monitors the probe position and vibrational amplitude to obtain topographical and other property information. Accurate topographical information can be obtained even for very fragile surfaces. Optimum resolution is about 50 Å lateral and <1 style="font-weight: bold;">Lateral Force Microscopy - This mode measures the lateral deflection of the probe cantilever as the tip is scanned across the sample in contact mode. Changes in lateral deflection represent relative frictional forces between the probe tip and the sample surface.

Phase Detection Microscopy With the system operating in Tapping mode, the cantilever oscillation is damped by interaction with the sample surface. The phase lag between the drive signal and actual cantilever oscillation is monitored. Changes in the phase lag indicate variations in the surface properties, such as viscoelasticity or mechanical properties. A phase image, typically collected simultaneously with a topographical image, maps the local changes in material’s physical or mechanical properties.

Magnetic Force Microscopy - This mode images local variations in the magnetic forces at the sample’s surface. The probe tip is coated with a thin film of ferromagnetic material that will react to the magnetic domains on the sample surface. The magnetic forces between the tip and the sample are measured by monitoring cantilever deflection while the probe is scanned at a constant height above the surface. A map of the forces shows the sample’s natural or applied magnetic domain structure.

Life-Cycle Analysis

The abbreviation LCA if used for both life-cycle analysis and for life-cycle assessment. However, they are two different concepts: life-cycle analysis is the scientific and technical analysis of impacts associated with a product or a system, while life-cycle assessment is the political evaluation based upon the analysis.

The need for incorporating study of environmental impacts in all assessment work performed in our societies, from consumer product evaluation to long-term planning decisions, is increasingly being accepted. Energy systems were among the first to be subjected to LCA, trying to identify environmental impacts and social impacts related e.g. to health, or in other words to include in the analysis impacts that have not traditionally been reflected in prices paid in the marketplace. This focuses on the sometimes huge difference between direct cost and the full cost, including what are termed externalities: those social costs that are not incorporated in market prices. It is seen as the role of societies (read governments) to make sure that the indirect costs are not neglected in consumer choices or decision-making processes related to planning in a society. The way externalities are included will depend on the political preferences. Possible avenues range from taxation to legislative regulation.

Life-cycle analysis is a tool suited for assisting planners and decisionmakers in performing the necessary assessments related to external costs. The LCA method aims at assessing all direct and indirect impacts of a technology, whether a product, an industrial plant, a system or an entire sector of society. LCA incorporates impacts over time, including impacts deriving from materials or facilities used to manufacture tools and equipment for the process under study, and it includes final disposal of equipment and materials, whether involving reuse, recycling or waste disposal. The two important characteristics of LCA are:

• Inclusion of “cradle to grave” impacts
• Inclusion of indirect impacts imbedded in materials and equipment

The ideas behind LCA were developed during the 1970s, and went under different names such as “total assessment”, “including externalities”, or “least cost planning”. Some of the first applications of LCA were in the energy field, including both individual energy technologies and entire energy supply systems. It was soon realised that the procurement of all required data was a difficult problem. As a result, the emphasis went towards LCA applied to individual products, where the data handling seemed more manageable. However, it is still a very open-ended process, because manufacture of say a milk container requires both materials and energy, and to assess the impacts associated with the energy input anyway calls for an LCA of the energy supply system. Only as the gathering of relevant data has been ongoing for a considerable time, has it become possible to perform credible LCA’s.

Product LCA has in recent years been promoted by organisations such as SETAC (Consoli et al., 1993) and several applications have appeared over recent years (e.g. Mekel and Huppes, 1990; Pommer et al., 1991; Johnson et al., 1994; DATV, 1995). Site− and technology− specific LCA of energy systems have been addressed by the European Commission (1995f) and by other recent projects (Petersen, 1991; Inaba et al., 1992; Kato et al, 1993; Meyer et al., 1994; Sørensen and Watt, 1993, Sørensen, 1994b; Yasukawa et al. 1996; Sørensen, 1995a, 1996c; Kuemmel et al., 1997). Methodological issues have been addressed by Baumgartner (1993); Sørensen (1993, 1995b, 1996b, 1997b); Engelenburg and Nieuwlaar (1993) and energy system-wide considerations by Knöepfel (1993); Kuemmel et al. (1997) and Sørensen (1997c), the latter with emphasis on greenhouse gas emission impacts.