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SEM/EDX analysis
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SEM/EDX analysis
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Image
Published: 01 November 2007
Fig. 10.52 Optical micrograph showing typical longitudinal cross section at the crown bead of the 312 waterwall overlay after about 6.5 years of service in a supercritical unit. The corrosion scales were chromium-rich oxides as identified by SEM/EDX analysis. Courtesy of Welding Services Inc.
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Image
in Waste-to-Energy Boilers and Waste Incinerators
> High-Temperature Corrosion and Materials Applications
Published: 01 November 2007
of the corrosion pits. SEM/EDX analysis on the corrosion products in one of the surface pits is summarized in Fig. 12.14 .
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Image
Published: 01 November 2007
Fig. 14.15 Type 304H tested in air + 4CO 2 + 8H 2 O at 610 °C (1130 °F) under the strain rate of 3 × 10 –8 /s with about 2% strain, showing preferential oxidation penetration (the authors referred to as ″cracking″). SEM/EDX analysis showed the oxide in area A was Fe-3Cr-4Si-0.5Mo, in area B
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Image
Published: 01 November 2007
and the EDX analysis of nitrides. Results of the semiquantitative EDX analysis (at.%) on internal aluminum nitrides are summarized as: Phase 1 41.5% Al, 24.7% Ni, 10.6% Cr, 6.8% Fe, 5.5% Ti, and 10.0% N Phase 2 58.0% Al, 13.1% Ni, 6.1% Cr, 3.6% Fe, 0.8% Ti, and 17.3% N
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Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110447
EISBN: 978-1-62708-247-1
... examples of the application of Auger and SEM-EDX. For Auger this is determination of oxide thickness and for SEM-EDX some examples of new applications in a dedicated section on particle analysis. Within NXP, all the techniques are available, but they are dispersed over 3 labs in Europe and US...
Abstract
There are several analytical methods available that can be used in-line on whole wafers as well as off-line on de-processed products that are returned from the field. These techniques are surface analytical techniques that can be used to characterize the bulk of the material. The main six methods used in semiconductor industry are: Auger spectroscopy, dynamic secondary ion mass spectroscopy, time of flight static secondary ion mass spectroscopy (ToF-SIMS), X-ray photoelectron spectroscopy, scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX), and transmission electron microscope-EDX. This review specifically addresses ToF-SIMS and describes some typical examples of the application of Auger and SEM-EDX.
Image
in Frontside Sample Preparation
> Microelectronics Failure Analysis<subtitle>Desk Reference</subtitle>
Published: 01 November 2019
Figure 9 Thinned capacitor location of greatest disturb to the monitored leakage and the correct position to move to SEM with EDX analysis.
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Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2007
DOI: 10.31399/asm.tb.htcma.t52080249
EISBN: 978-1-62708-304-1
... °C (1650 °F) with 50 ppm sea salt being injected into the combustion gas stream. Scanning electron microscopy with energy-dispersive x-ray spectroscopy (SEM/EDX) analysis showed that both nickel aluminides exhibited porous nickel or nickel-rich oxides with nickel sulfide penetrating through...
Abstract
This chapter examines the hot corrosion resistance of various nickel- and cobalt-base alloys in gas turbines susceptible to high-temperature (Type I) and low-temperature (Type II) hot corrosion. Type I hot corrosion is typically characterized by a thick, porous layer of oxides with the underlying alloy matrix depleted in chromium, followed (below) by internal chromium-rich sulfides. Type II hot corrosion is characterized by pitting with little or no internal attack underneath. As the chapter explains, chromium additions make alloys more resistant to all types of hot corrosion attacks.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2007
DOI: 10.31399/asm.tb.htcma.t52080259
EISBN: 978-1-62708-304-1
... at different locations were analyzed by energy dispersive x-ray spectroscopy (EDX) with the results summarized as: 1: 1.1% S, 0.7% Al, 0.8% Si, 0.6% Mn, 95% Fe, and trace elements 2: 0.8% S, 0.3% Al, 0.6% Si, 0.5% Cl, 0.5% Ca, 1.9% Zn, 94% Fe, and trace elements 3: 13.4% S, 0.8% Al, 0.4% Si, 0.8% Mn...
Abstract
This chapter discusses material-related problems associated with coal-fired burners. It explains how high temperatures affect heat-absorbing surfaces in furnace combustion areas and in the convection pass of superheaters and reheaters. It describes how low-NOx combustion technology, intended to reduce NOx emissions, accelerates tube wall wastage. It also covers circumferential cracking in furnace waterwalls, thermal fatigue cracking induced by waterlances and water cannons, superheater-reheater corrosion, and erosion in fluidized-bed boilers.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 September 2008
DOI: 10.31399/asm.tb.fahtsc.t51130351
EISBN: 978-1-62708-284-6
... features of the fracture surface as observed by the SEM. (a) Overall view of the fracture surface (111 μm). (b) Intergranular fracture observed on the fracture surface (10 μm) A hydrogen analysis was conducted on the MLG lever attach pin before and after baking for 24 h at 190 °C (375 °F...
Abstract
This chapter presents various case histories that illustrate a variety of failure mechanisms experienced by the high-strength steel components in aerospace applications. The components covered are catapult holdback bar, AISI 420 stainless steel roll pin, main landing gear (MLG) lever, inboard flap hinge bolt, nose landing gear piston axle, multiple-leg aircraft-handling sling, aircraft hoist sling, internal spur gear, and MLG axle. In addition, the chapter provides information on full-scale fatigue testing, nondestructive testing, and failure analysis of fin attach bolts.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110144
EISBN: 978-1-62708-247-1
... and reduced to just a few microns per pass in figure 9 , as the leakage became increasingly chaotic. With about 10μm of remaining plastic, the thinning was halted and EDX analysis performed in the SEM. See figure 10 . Silver was found on the ceramic body of the capacitor sidewall. Figure 9 Thinned...
Abstract
The orientation of the devices within a package determine the best chosen approach for access to a select component embedded in epoxy both in package or System in Package and multi-chip module (MCM). This article assists the analyst in making decisions on frontside access using flat lapping, chemical decapsulation, laser ablation, plasma reactive ion etching (RIE), CNC based milling and polishing, or a combination of these coupled with optical or electrical endpoint means. This article discusses the general characteristics, advantages, and disadvantages of each of these techniques. It also presents a case study illustrating the application of CNC milling to isolate MCM leakage failure.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 August 2005
DOI: 10.31399/asm.tb.horfi.t51180151
EISBN: 978-1-62708-256-3
... done with an SEM. An SEM has the advantage over light microscopy because of the large depth of field and very high magnifications attainable, typically 5000 to 10,000×. In addition, SEMs are often equipped with microanalytical capabilities, for example, energy-dispersive x-ray (EDX) spectroscopes...
Abstract
This appendix focuses on procedures, techniques, and precautions associated with the investigation and analysis of metallurgical failures that occur in service. It describes the steps of an orderly failure analysis from collecting and examining samples to performing mechanical and nondestructive tests, preparing and examining fractographs and micrographs, determining failure mode, writing the report, and developing follow-up recommendations. It also examines the fundamental mechanisms of failure, why they occur, and how to identify them by their characteristic features.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 March 2012
DOI: 10.31399/asm.tb.pdub.t53420239
EISBN: 978-1-62708-310-2
... microanalysis (EPMA) is another important technique for phase diagram determination. It is essentially a dedicated SEM with wavelength dispersive spectrometers (WDS) attached. As an elemental analysis technique, it uses a focused beam of high-energy electrons (5 to 30 KeV) in the SEM to impinge on a sample...
Abstract
This chapter discusses some of the methods and measurements used to construct phase diagrams. It explains how cooling curves were widely used to determine phase boundaries, and how equilibrated alloys examined under controlled heating and cooling provide information for constructing isothermal and vertical sections as well as liquid projections. It also explains how diffusion couples provide a window into local equilibria and identifies typical phase diagram construction errors along with problems stemming from phase-boundary curvatures and congruent transformations.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110413
EISBN: 978-1-62708-247-1
... and large sample areas can be scanned. Under the right circumstances SEM can achieve 1 nm resolution which is very close to TEM and AFM. It is also relatively simple and inexpensive to add an energy dispersive x-ray detector (EDX) to a SEM which then provides a chemical micro-analysis capability (see...
Abstract
This article provides an overview of how to use the scanning electron microscope (SEM) for imaging integrated circuits. The discussion covers the principles of operation and practical techniques of the SEM. The techniques include sample mounting, sample preparation, sputter coating, sample tilt and image composition, focus and astigmatism correction, dynamic focus and image correction, raster alignment, and adjusting brightness and contrast. The article also provides information on achieving ultra-high resolution in the SEM. It concludes with information on the general characteristics and applications of environmental SEM.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110434
EISBN: 978-1-62708-247-1
... detector scanning transmission electron microscope-EDS silicon drift detector wavelength dispersive X-ray detector Introduction By far the most common micro-analytical technique in the failure analysis laboratory is energy dispersive x-ray spectroscopy, known as EDX or EDS. It is commonly...
Abstract
This article provides an overview of the most common micro-analytical technique in the failure analysis laboratory: energy dispersive X-ray spectroscopy (EDS). It discusses the general characteristics, advantages, and disadvantages of some of the X-ray detectors attached to the scanning electron microscope chamber including the lithium-drifted EDS detector, silicon drift detector (SDD), and wavelength dispersive X-ray detector. The article then provides information on qualitative and quantitative X-ray analysis programs followed by a discussion on EDS elemental mapping. The discussion includes a comparison of scanning transmission electron microscope-EDS elemental mapping and mapping with an SDD. A brief section is devoted to the discussion on the artifacts that occur during X-ray mapping.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2007
DOI: 10.31399/asm.tb.htcma.t52080067
EISBN: 978-1-62708-304-1
... immediately below, followed by internal nitrides underneath the denuded zone. (b) Optical micrograph at higher magnification showing internal nitrides. (c) SEM (backscattered electron image) showing internal aluminum nitrides and the EDX analysis of nitrides. Results of the semiquantitative EDX analysis...
Abstract
Oxidation usually dominates high-temperature corrosion reactions, but under certain conditions, some alloys may be affected by nitridation as well. This chapter explains why nitridation occurs and how it attacks various metals, in some cases, penetrating deeper than oxidation. It provides images and data describing the nitridation process and its effects on metals and alloys in high-temperature air as well as NH3-H2O, NH3 and H2-N2-NH3, and N2 environments. It also includes test data showing that nitridation is more severe in a nitrogen atmosphere than an ammonia environment at 1090 °C (2000 °F).
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110209
EISBN: 978-1-62708-247-1
... the packaging material surrounding the hot spot; subsequently, LIT imaging was performed to better localize the hot spot ( Fig. 10b ). Cross sectioning was then performed at the hot-spot area. SEM/EDX investigations identified an Al-splinter as the root cause of the defect. Fig. 10 (a) LIT results...
Abstract
Many defects generate excessive heat during operation; this is due to the power dissipation associated with the excess current flow at the defect site. There are several thermal detection techniques for failure analysis and this article focuses on infrared thermography with lock-in detection, which detects an object's temperature from its infrared emission based on blackbody radiation physics. The basic principles and the interpretation of the results are reviewed. Some typical results and a series of examples illustrating the application of this technique are also shown. Brief sections are devoted to the discussion on liquid-crystal imaging and fluorescent microthermal imaging technique for thermal detection.
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2019
DOI: 10.31399/asm.tb.mfadr7.t91110563
EISBN: 978-1-62708-247-1
... vertically stuck beams on MEMS accelerometer. Diagnosing stiction is straightforward with optical or SEM inspection, but finding the root cause requires knowing the history of the part: shocks during handling, analysis, or shipping have the potential to stick and/or release MEMS structures. This must...
Abstract
This chapter discusses the various failure analysis techniques for microelectromechanical systems (MEMS), focusing on conventional semiconductor manufacturing processes and materials. The discussion begins with a section describing the advances in integration and packaging technologies that have helped drive the further proliferation of MEMS devices in the marketplace. It then shows some examples of the top MEMS applications and quickly discusses the fundamentals of their workings. The next section describes common failure mechanisms along with techniques and challenges in identifying them. The chapter also provides information on the testing of MEMS devices. It covers the two common challenges in sample preparation for MEMS: decapping, or opening up the package, without disturbing the MEMS elements; and removing MEMS elements for analysis. Finally, the chapter discusses the aspects of failure analysis techniques that are of particular interest to MEMS.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2007
DOI: 10.31399/asm.tb.htcma.t52080379
EISBN: 978-1-62708-304-1
...% strain, showing preferential oxidation penetration (the authors referred to as ″cracking″). SEM/EDX analysis showed the oxide in area A was Fe-3Cr-4Si-0.5Mo, in area B was Fe-29Cr-5Ni-0.8Mo-0.8Si, and in area C was Fe-37Cr-21Ni-1.5Si. Source: Ref 10 Rorbo ( Ref 11 ) reported that the external...
Abstract
This chapter discusses two damage mechanisms in which stress plays a major role. In the one case, stress causes cracks in the oxide scale on metals, leading to preferential corrosion attack. An example from industry of this type of failure is the circumferential cracking that occurs on the waterwall tubes of supercritical coal-fired boilers fired under low NOx combustion conditions, conducive to the production of sulfidizing environments. In the other case, stress contributes to brittle fracture in the form of intergranular cracking. The phenomenon, which is known by various names, typically occurs at the lower end of the intermediate temperature range and has been observed in ferritic steels, stainless steels, Fe-Ni-Cr alloys, and nickel-base alloys, as described in the chapter.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 November 2007
DOI: 10.31399/asm.tb.htcma.t52080005
EISBN: 978-1-62708-304-1
... months of service ( Ref 30 ). The oxide scales were analyzed by scanning electron microscopy/energy-dispersive x-ray spectroscopy (SEM/EDX) analysis; the results are shown in Fig. 3.21 . The analysis showed that the outermost oxide layer was essentially iron oxides with very little chromium. Thus...
Abstract
Many metallic components, such as retorts in heat treat furnaces, furnace heater tubes and coils in chemical and petrochemical plants, waterwalls and reheater tubes in boilers, and combustors and transition ducts in gas turbines, are subject to oxidation. This chapter explains how oxidation affects a wide range of engineering alloys from carbon and Cr-Mo steels to superalloys. It discusses the kinetics and thermodynamics involved in the formation of oxides and the effect of surface and bulk chemistry. It provides oxidation data for numerous alloys and intermetallics in terms of weight gain, metal loss, depth of attack, and oxidation rate. It also discusses the effect of metallurgical and environmental factors such as oxygen concentration, high-velocity combustion gas streams, chromium depletion and breakaway, component thickness, and water vapor.
Book Chapter
Series: ASM Technical Books
Publisher: ASM International
Published: 01 September 2008
DOI: 10.31399/asm.tb.fahtsc.t51130151
EISBN: 978-1-62708-284-6
... of a component during heat treatment or in service. The failure analyst uses these seven items as a guide in a failure analysis. This chapter deals specifically with improper casting projects and those features that originated in the casting process itself, including porosity (generated by the presence of gas...
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