This article discusses the operating principles, advantages, and limitations of scanning electron microscopy, atomic force microscopy, x-ray photoelectron spectroscopy, and secondary ion mass spectroscopy that are used to analyze the surface chemistry of plastics.

The paper discusses the analysis of a coating defect on a high phosphorus electroless nickel (Ni-11 wt. % P) deposit plated on an aluminum alloy substrate. Preliminary investigations had indicated that the elongated defects were possibly caused by the entrapment of long fibers or particles during the plating. The possible sources of fibers were identified. The SEM/EDS analysis of fibers collected from the air duct filters correlated very well with the defect shape and the EDS profile collected from under the defect site. It appears that the fibers from air duct filters directly above the plating line were blown into the plating tank and getting co-deposited. The paper describes the step-by-step analysis of the defect that led to successful identification of the root cause of the defect.

Several crankshaft failures occurred in equipment that was being used in logging operations in subzero temperatures. Failure usually initiated at a cracked pin oil hole, and the failure origin was approximately 7.6 mm (0.3 in.) from the shaft surface. The holes were produced by gun drilling, giving rise to surface defects. The fracture surface was characteristic of fatigue in that it was flat, relatively shiny, and exhibited beach marks. The crack surface was at a 45 deg angle to the axis of the shaft, indicating dominant tensile stresses. The material was the French designation AFNOR 38CD4 (similar to AISI type 4140H) and was in the quenched-and-tempered condition, with a yield strength of about 760 MPa (110 ksi). It was treated to have compressive surface stresses, and the prior-austenite grain size was ASTM 8. Analysis (visual inspection, stress analyses, and macrographs) supported the conclusion that failure was caused by fatigue stress caused by surface defects in the oil holes. Recommendation includes drilling the oil holes by a technique that essentially eliminates surface defects.

An automobile manufacturer rejected several 1035 steel stub axles because of what appeared to be short longitudinal cracks in the surfaces of the pins. The cracks were found when six axles were examined for defects by magnetic-particle inspection. However, metallographic examination showed that these lines were not cracks but slag inclusions at and immediately below the surface. Analysis (visual inspection, metallographic examination, and 100x/500x magnetic-particle inspection) supported the conclusions that the inclusions consisted of pieces of fireclay from channel brick that were flushed into the ingot mold. Although no true cracks were present, rejection of the stub axles was nevertheless justified. Slag streaks could reduce the strength of the stub axles and lead to the formation of fatigue fractures during operation. No recommendations were made.

A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel-phosphorus side of the clad bimetal onto an epoxy film, so that the end product contained nickel-phosphorus sandwiched between copper and epoxy, with a chromate conversion layer on the epoxy side of the nickel-phosphorus. Peel testing showed abnormally low adhesion strength for the bad batch of peel test samples. Comparison with normal-strength samples using XPS indicated an 8.8% Na concentration on the surface of the bad sample; the good example contained less than 1% Na on the surface. After 15 min of argon ion etching, depth profiling showed high concentrations of sodium were still evident, indicating that the sodium was present before the chromate conversion treatment was performed. A review of the manufacturing procedures showed that sodium hydroxide was used as a cleaning agent before the chromate conversion coating. Failure cause was that apparently the sodium hydroxide had not been properly removed during water rinsing. Thus, recommendation was to modify that stage in the processing.

This article covers the three most popular techniques used to characterize the very outermost layers of solid surfaces: Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Some of the more important attributes are listed for preliminary insight into the strengths and limitations of these techniques for chemical characterization of surfaces. The article describes the basic theory behind each of the different techniques, the types of data produced from each, and some typical applications. Also discussed are the different types of samples that can be analyzed and the special sample-handling procedures that must be implemented when preparing to do failure analysis using these surface-sensitive techniques. Data obtained from different material defects are presented for each of the techniques. The examples presented highlight the typical data sets and strengths of each technique.

This article provides information on the chemical characterization of surfaces by Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). It describes the basic theory behind each of these techniques, the types of data produced from each, and some typical applications. The article explains the strengths of AES, XPS, and TOF-SIMS based on data obtained from the surface of a slightly corroded stainless steel sheet.

The damage to a screw on the head of a 1.8 liter personal car engine was nucleated as the result of common disadvantageous environmental influences and reversed loads leading to corrosion fatigue.

Cracking occurred in an ASME SB166 Inconel 600 safe-end forging on a nuclear reactor coolant water recirculation nozzle while it was in service. The safe-end was welded to a stainless-steel-clad carbon steel nozzle and a type 316 stainless steel transition metal pipe segment. An Inconel 600 thermal sleeve was welded to the safe-end, and a repair weld had obviously been made on the outside surface of the safe-end to correct a machining error. Initial visual examination of the safe-end disclosed that the cracking extended over approximately 85 deg of the circular circumference of the piece. Investigation (visual inspection, on-site radiographic inspection, limited ultrasonic inspection, chemical analysis, 53x metallographic cross sections and SEM images etched in 8:1 phosphoric acid) supported the conclusion that the cracking mechanism was intergranular SCC. No recommendations were made.