This article presents best practices for the metallographic preparation of specimens produced via thermal spray coating methods. It outlines typical metallographic preparation process flow, highlighting important considerations for obtaining a clear and representative specimen suitable for characterization via examination techniques, such as optical or electron microscopy. The process flow includes preliminary resin infiltration, sectioning, mounting, grinding, and polishing. To aid in the identification and resolution of common issues during subsequent specimen analysis, the article presents common issues, along with causes and mitigation strategies. It describes the processes involved in the interpretation of the thermal spray coating microstructure.

Thermal barrier coatings (TBCs) are applied using thermal spray coating (TSC) processes to components that are internally cooled and operated in a heated environment. The TSC microstructures are prone to interactions with common metallographic procedures that may result in artifacts and misinterpretation of the TSC microstructure. This article aims to aid in identifying metallographic TSC artifacts, specifically in the air plasma spray zirconia-based TBC, including both of its common constituents, the bond coating and the top coating. Artifacts that result from specific sectioning and mounting practices, as well as from different polishing times, are presented. Additionally, the article discusses the factors in optical microscopy and scanning electron microscopy that affect microstructure interpretation.

Abradable coatings (such as Ni-4Cr-4Al/bentonite) are used throughout jet engines, primarily as sacrificial coatings into which moving components wear. This article presents the Accepted Practice for sample preparation of abradable coatings for metallographic analysis, based on round robin testing by several laboratories.

Molybdenum thermal spray coatings are used in aerospace and other industries for wear resistance applications. Metallographic sample preparation of molybdenum coatings presents unique challenges. The purpose of the investigation described in this article is to determine Accepted Practices for sample preparation to better understand the process related microstructures of thermal spray molybdenum powders. The committee followed a round robin approach to assess metallographic sample preparation by a variety of laboratories. The article summarizes the results of the committee’s work.

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.

This chapter discusses the practices and procedures used to reveal and record macrostructural features such as hardening depth, weld thickness, crack size, porosity, hot folds, and machining and tooling marks. It provides information on sectioning, sample location, orientation, surface grinding, and etching. It describes macrographic etchants and the features they reveal along with common etching problems and how to avoid them. It explains how to evaluate etching results and how they can be improved using remedial processes such as light grinding. It also discusses photographic reproduction, lighting, and image enhancement techniques.

This chapter explains how to prepare material samples for optical microscopy, the most common method for characterizing the microstructure of cast iron and steel. It provides information on sectioning, mounting, polishing, etching, and recording. It describes the nature of surface roughness, the factors that contribute to it, and its effect on image quality. It discusses the use of fixturing and holding devices, includes photographic examples of polishing defects and drying marks, and provides an overview of micrographic etchants and the features they reveal. It also describes the steps involved in replicating part surfaces.

This chapters discusses the basic steps in the failure analysis process. It covers examination procedures, selection and preservation of fracture surfaces, macro and microfractography, metallographic analysis, mechanical testing, chemical analysis, and simulated service testing.

This chapter discusses composite testing procedures, including tension, compression, shear, flexure, and fracture toughness testing as well as adhesive shear, peel, and honeycomb flatwise tension testing. It also discusses specimen preparation, environmental conditioning, and data analysis.

Specimen preparation is the first step that determines the quality of the microstructural information that can be obtained using optical microscopy. This chapter describes the sample preparation methods that are applicable to most types of composite materials containing short discontinuous or continuous fibers. The sample preparation methods cover documentation and labeling of samples, sectioning the composite, clamp-mounting composite samples, mounting composite samples in casting resins, and the addition of contrast dyes to casting resins. Information on the molds used for mounting composite materials is provided. The steps recommended to achieve a good mounted specimen without voids or specimen pull-out are also described. The chapter discusses the processes for clamping mounted composite samples in automated polishing heads and mounting composite materials for hand polishing. A summary of the mounting technique is also included.

Rough grinding and polishing of mounted specimens are required to prepare the composite sample for optical analysis. This chapter describes these techniques for preparing composite materials. First, it provides information on grinding and polishing equipment and describes the processes and process variables for sample preparation. Then, the chapter discusses the processes of abrasive sizing for grinding and rough polishing. Next, it provides a summary of grinding methods, rough polishing, and final polishing. Finally, information on common polishing artifacts that can result from any of the steps is provided.

The most common methods for preparing polymeric composites for microscopic analysis can be used for most fiber-reinforced composite materials. There are, however, a few composite materials that require special preparation techniques. This chapter discusses the processes involved in the preparation of titanium honeycomb composites, boron fiber composites, titanium/polymeric composite hybrids, and uncured prepreg materials.

Transmitted-light methods reveal more details of the morphology of fiber-reinforced polymeric composites than are observable using any other available microscopy techniques. This chapter describes the various aspects relating to the selection and preparation of ultrathin-section specimens of fiber-reinforced polymeric composites for examination by transmitted-light microscopy techniques. The preparation steps covered are a selection of the rough section, preparation of the rough section for preliminary mounting, grinding and polishing the primary-mount first surface, mounting the first surface on a glass slide, and preparing the second surface (top surface). The optimization of microscope conditions and analysis of specimens by microscopy techniques are also covered. In addition, examples of composite ultrathin sections that are analyzed using transmitted-light microscopy contrast methods are shown throughout.

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.

This appendix contains figures that illustrate specimen orientation and crack plane codes for rolled plate, drawn bars, and hollow cylinders.

This chapter instructs the metallographer on the basic skills required to prepare a polished metallographic specimen. It is organized in a chronological sequence starting with the information-gathering process on the material being investigated, then moving on to sectioning, mounting, grinding, and polishing processes, and ending with methods used to properly store metallographic specimens. The discussion covers the preparation procedures, the materials being investigated, and equipment used to perform these procedures.

Corrosion testing and monitoring are powerful tools in the fight to control corrosion. This chapter provides a general overview of three major categories of corrosion tests, namely laboratory tests, pilot-plant tests, and field tests. It begins with brief sections describing the purposes of corrosion tests, the logical steps in a test program, and the preparation and cleaning of test specimens. The focus then moves on to discuss the types and applications of these test categories and the associated evaluation procedures. Excluding electrochemical tests which are addressed separately in this chapter, the other laboratory tests covered under this category are simulated atmosphere tests, salt-spray tests, and immersion tests. Only corrosion testing in the atmosphere is discussed in the section on field tests. Corrosion monitoring techniques are finally considered, covering the characteristics of corrosion monitoring techniques, the factors to be considered in selecting a corrosion-monitoring method, and the strategies in corrosion monitoring.

This chapter explains how to prepare metallographic samples for light microscopy and how to anticipate and avoid related problems. It describes standard practices and procedures for sectioning, mounting, grinding, and polishing and identifies common defects along with their causes and cures. It also provides recommendations for handling specific materials and addresses safety concerns.