The analysis of composite materials using optical microscopy is a process that can be made easy and efficient with only a few contrast methods and preparation techniques. This chapter is intended to provide information that will help an investigator select the appropriate microscopy technique for the specific analysis objectives with a given composite material. The chapter opens with a discussion of macrophotography and microscope alignment, and then goes on to describe various illumination techniques that are useful for specific analysis requirements. These techniques include bright-field illumination, dark-field illumination, polarized-light microscopy, interference and contrast microscopy, and fluorescence microscopy. The chapter also provides a discussion of sample preparation materials such as dyes, etchants, and stains for the analysis of composite materials using optical microscopy.

This chapter discusses the tools and techniques of light microscopy and how they are used in the study of materials. It reviews the basic physics of light, the inner workings of light microscopes, and the relationship between resolution and depth of field. It explains the difference between amplitude and optical-phase features and how they are revealed using appropriate illumination methods. It compares images obtained using bright field and dark field illumination, polarized and cross-polarized light, and interference-contrast techniques. It also discusses the use of photometers, provides best practices and recommendations for photographing structures and features of interest, and describes the capabilities of hot-stage and hot-cell microscopes.

Microstructural analysis of the composite matrix is necessary to understand the performance of the part and its long-term durability. This chapter focuses on the microstructural analysis of engineering thermoplastic-matrix composites and the influence of cooling rate and nucleation on the formation of spherulites in high-temperature thermoplastic-matrix carbon-fiber-reinforced composites. It also describes the microstructural analysis of a bio-based thermosetting-matrix natural fiber composite system.

As fiber-reinforced polymeric composites continue to be used in more damage-prone environments, it is necessary to understand the response of these materials when subjected to impact from foreign objects. This chapter provides an overview of the analysis methods for impact-damaged composites. It discusses the causes and effects of various failure mechanisms in composite materials. The failure mechanisms covered are brittle-matrix composite failure, tough-matrix composite failure, thermoplastic-matrix composite failure mechanisms, untoughened thermoset-matrix composite failure mechanisms, toughened thermoset-matrix composite failure mechanisms, particle interlayer-toughened composite failure mechanisms, and dispersed-phase, rubber-toughened thermoset-matrix composite failure mechanisms.

The formation of microcracks in composite materials may arise from static-, dynamic-, impact-, or fatigue-loading situations and also by temperature changes or thermal cycles. This chapter discusses the processes involved in the various methods for the microcrack analysis of composite materials, namely bright-field analysis, polarized-light analysis, contrast dyes analysis, and dark-field analysis. The analysis of microcracked composites using epi-fluorescence is also covered. In addition, the chapter describes the procedures for the determination and recording of microcracks in composite materials.

Moore's Law has driven many degree circuit features below the resolving capability of optical microscopy. Yet the optical microscope remains a valuable tool in failure analysis. This article describes the physics governing resolution and useful techniques for extracting the small details. It begins with the basic microscope column and construction. The article discusses microscope adjustments, brightfield and darkfield illumination, and microscope concepts important to liquid crystal techniques. It also discusses solid immersion lenses, infrared and ultraviolet microscopy and concludes with laser microscopy techniques such as thermal induced voltage alteration and external induced voltage alteration.

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 chapter describes the methods and equipment applicable to metallographic studies and discusses the preparation of specimens for examination by light optical microscopy. Five major operations for preparation of metallographic specimens are discussed: sectioning, mounting, grinding, polishing, and etching. The discussion covers their basic principles, advantages, types, and applications, as well as the equipment setup. The chapter includes tables that list etchants used for microscopic examination. It also provides information on microscopic examination, microphotography, and the effects of grain size on the structural properties of the material.

Analyzing the structure of composite materials is essential for understanding how the part will perform in service. Assessing fiber volume variations, void content, ply orientation variability, and foreign object inclusions helps in preventing degradation of composite performance. This chapter describes the optical microscopy and bright-field illumination techniques involved in analyzing ply terminations, prepreg plies, splices, and fiber orientation to provide the insight necessary for optimizing composite structure and performance.

This chapter provides a general description of materials and methods for manufacturing high-performance composites. The materials covered are polymer matrices and prepreg materials and the methods include infusion processes, composite-toughening methods, matrix-toughening methods, and dispersed-phase toughening. In addition, the chapter provides information on interlayer-toughened composites and honeycomb or foam structure composite materials. It also discusses the processes in optical microscopy of composite materials.

The honeycomb sandwich structure composite is a very efficient and complex structure widely used in the aircraft industry. Honeycomb-cored sandwich panels increase part stiffness at a lower weight than monolithic composite materials. This chapter describes the analysis of the intermingling of the film adhesive/prepreg resin system. It discusses the causes and effects of honeycomb core movement, which results in core crush. The chapter also explains the formation of a void in honeycomb composites and the failure mechanisms in honeycomb sandwich structure composites.

Lightning damage in polymer composites, as in metal structures, is manifested by damage at both the macroscopic or visual level and within the material microstructure. In addition to visual damage assessment, non-destructive inspection techniques are employed to detect damage within the composite part. This chapter describes the macroeffects of a lightning strike on composites and discusses the methods involved in the assessment of microstructural damage in composites.

This chapter explains how to achieve accurate, sharp delineation of the microstructure of metals using appropriate etching and contrasting techniques. It covers a variety of methods, including chemical etching, heat tinting, gas contrasting, vapor deposition, magnetic etching, ion bombardment, and dislocation etch pitting.

Intermetallic phase precipitates in aluminum alloys can often be identified without resorting to chemical analysis. Very often the determination can be made based on the shape, color, and refractive properties of the particular phase. This chapter explains how these visual attributes can be observed using metallographic techniques. It describes, and in many cases illustrates, the characteristic shapes, colors, and optical properties associated with aluminum alloy intermetallic phases and how they can be enhanced through selective etching. It provides an atlas of microstructures comparing the effects of selective etching procedures on various phase constituents in cast aluminum-silicon alloys. The compilation of images demonstrates the use of two types of reagents: those that reveal discontinuities in crystal orientation and grain boundaries, and those that reveal differences in chemical composition.

The second-generation composite materials were added to increase the strain to failure of the primary phase and/or create a dispersed second phase, thereby enhancing the fracture toughness of the thermosetting matrix. These matrices offered novel design capabilities for composites in a variety of aircraft applications. To improve the damage tolerance of composite materials even further, an engineering approach to toughening was used to modify the highly stressed interlayer with either a tougher material or through the use of preformed particles, leading to the third generation of composite materials. This chapter discusses the development, processes, application, advantages, and disadvantages of dispersed-phase toughening of thermoset matrices. Information on the processes of particle interlayer toughening of composite materials is also included.

This article reviews the basic physics behind active photon injection for local photocurrent generation in silicon and thermal laser stimulation along with standard scanning optical microscopy failure analysis tools. The discussion includes several models for understanding the local thermal effects on metallic lines, junctions, and complete devices. The article also provides a description and case study examples of multiple photocurrent and thermal injection techniques. The photocurrent examples are based on Optical Beam-Induced Current and Light-Induced Voltage Alteration. The thermal stimulus examples are Optical Beam-Induced Resistance Change/Thermally-Induced Voltage Alteration and Seebeck Effect Imaging. Lastly, the article discusses the application of solid immersion lenses to improve spatial resolution.

This chapter explains how to safely prepare beryllium alloy samples for metallographic analysis. It describes grinding, polishing, and etching procedures in detail. It also discusses the identification of major and minor constituents and the general appearance of beryllium microstructure.

Scanning Probe Microscope (SPM) has an increasing important role in the development of nanoscale semiconductor technologies. This article presents a detailed discussion on various SPM techniques including Atomic Force Microscopy (AFM), Scanning Kelvin Probe Microscopy, Scanning Capacitance Microscopy, Scanning Spreading Resistance Microscopy, Conductive-AFM, Magnetic Force Microscopy, Scanning Surface Photo Voltage Microscopy, and Scanning Microwave Impedance Microscopy. An overview of each SPM technique is given along with examples of how each is used in the development of novel technologies, the monitoring of manufacturing processes, and the failure analysis of nanoscale semiconductor devices.