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Metallography is the study of the physical structure and components of metals, by using microscopy.
Ceramic and polymeric materials may also be prepared using metallographic techniques, hence the terms ceramography, plastography and, collectively, materialography.
The surface of a metallographic specimen is prepared by various methods of grinding, polishing, and etching. After preparation, it is often analyzed using optical or electron microscopy. Using only metallographic techniques, a skilled technician can identify alloys and predict material properties.
Mechanical preparation is the most common preparation method. Successively finer abrasive particles are used to remove material from the sample surface until the desired surface quality is achieved. Many different machines are available for doing this grinding and polishing, which are able to meet different demands for quality, capacity, and reproducibility.
A systematic preparation method is the easiest way to achieve the true structure. Sample preparation must therefore pursue rules which are suitable for most materials. Different materials with similar properties (hardness and ductility) will respond alike and thus require the same consumables during preparation.
Metallographic specimens are typically "mounted" using a hot compression thermosetting resin. In the past, phenolic thermosetting resins have been used, but modern epoxy is becoming more popular because reduced shrinkage during curing results in a better mount with superior edge retention. A typical mounting cycle will compress the specimen and mounting media to 4,000 psi (28 MPa) and heat to a temperature of 350 °F (177 °C). When specimens are very sensitive to temperature, "cold mounts" may be made with a two-part epoxy resin. Mounting a specimen provides a safe, standardized, and ergonomic way by which to hold a sample during the grinding and polishing operations.
After mounting, the specimen is wet ground to reveal the surface of the metal. The specimen is successively ground with finer and finer abrasive media. Silicon carbide abrasive paper was the first method of grinding and is still used today. Many metallographers, however, prefer to use a diamond grit suspension which is dosed onto a reusable fabric pad throughout the polishing process. Diamond grit in suspension might start at 9 micrometres and finish at one micrometre. Generally, polishing with diamond suspension gives finer results than using silicon carbide papers (SiC papers), especially with revealing porosity, which silicon carbide paper sometimes "smear" over. After grinding the specimen, polishing is performed. Typically, a specimen is polished with a slurry of alumina, silica, or diamond on a napless cloth to produce a scratch-free mirror finish, free from smear, drag, or pull-outs and with minimal deformation remaining from the preparation process.
After polishing, certain microstructural constituents can be seen with the microscope, e.g., inclusions and nitrides. If the crystal structure is non-cubic (e.g., a metal with a hexagonal-closed packed crystal structure, such as Ti or Zr) the microstructure can be revealed without etching using crossed polarized light (light microscopy). Otherwise, the microstructural constituents of the specimen are revealed by using a suitable chemical or electrolytic etchant.
Non-destructive surface analysis techniques can involve applying a thin film or varnish that can be peeled off after drying and examined under a microscope. The technique was developed by Pierre Armand Jacquet and others in 1957. [1]
Many different microscopy techniques are used in metallographic analysis.
Prepared specimens should be examined with the unaided eye after etching to detect any visible areas that have responded to the etchant differently from the norm as a guide to where microscopical examination should be employed. Light optical microscopy (LOM) examination should always be performed prior to any electron metallographic (EM) technique, as these are more time-consuming to perform and the instruments are much more expensive.
Further, certain features can be best observed with the LOM, e.g., the natural color of a constituent can be seen with the LOM but not with EM systems. Also, image contrast of microstructures at relatively low magnifications, e.g., <500X, is far better with the LOM than with the scanning electron microscope (SEM), while transmission electron microscopes (TEM) generally cannot be utilized at magnifications below about 2000 to 3000X. LOM examination is fast and can cover a large area. Thus, the analysis can determine if the more expensive, more time-consuming examination techniques using the SEM or the TEM are required and where on the specimen the work should be concentrated.
Light microscopes are designed for placement of the specimen's polished surface on the specimen stage either upright or inverted. Each type has advantages and disadvantages. Most LOM work is done at magnifications between 50 and 1000X. However, with a good microscope, it is possible to perform examination at higher magnifications, e.g., 2000X, and even higher, as long as diffraction fringes are not present to distort the image. However, the resolution limit of the LOM will not be better than about 0.2 to 0.3 micrometers. Special methods are used at magnifications below 50X, which can be very helpful when examining the microstructure of cast specimens where greater spatial coverage in the field of view may be required to observe features such as dendrites.
Besides considering the resolution of the optics, one must also maximize visibility by maximizing image contrast. A microscope with excellent resolution may not be able to image a structure, that is there is no visibility, if image contrast is poor. Image contrast depends upon the quality of the optics, coatings on the lenses, and reduction of flare and glare; but, it also requires proper specimen preparation and good etching techniques. So, obtaining good images requires maximum resolution and image contrast.
Most LOM observations are conducted using bright-field (BF) illumination, where the image of any flat feature perpendicular to the incident light path is bright, or appears to be white. But, other illumination methods can be used and, in some cases, may provide superior images with greater detail. Dark-field microscopy (DF), is an alternative method of observation that provides high-contrast images and actually greater resolution than bright-field. In dark-field illumination, the light from features perpendicular to the optical axis is blocked and appears dark while the light from features inclined to the surface, which look dark in BF, appear bright, or "self-luminous" in DF. Grain boundaries, for example, are more vivid in DF than BF.
Polarized light (PL) is very useful when studying the structure of metals with non-cubic crystal structures (mainly metals with hexagonal close-packed (hcp) crystal structures). If the specimen is prepared with minimal damage to the surface, the structure can be seen vividly in cross-polarized light (the optic axis of the polarizer and analyzer are 90 degrees to each other, i.e., crossed). In some cases, an hcp metal can be chemically etched and then examined more effectively with PL. Tint etched surfaces, where a thin film (such as a sulfide, molybdate, chromate or elemental selenium film) is grown epitaxially on the surface to a depth where interference effects are created when examined with BF producing color images, can be improved with PL. If it is difficult to get a good interference film with good coloration, the colors can be improved by examination in PL using a sensitive tint (ST) filter.
Another useful imaging mode is differential interference contrast (DIC), which is usually obtained with a system designed by the Polish physicist Georges Nomarski. This system gives the best detail. DIC converts minor height differences on the plane-of-polish, invisible in BF, into visible detail. The detail in some cases can be quite striking and very useful. If an ST filter is used along with a Wollaston prism, color is introduced. The colors are controlled by the adjustment of the Wollaston prism, and have no specific physical meaning, per se. But, visibility may be better.
DIC has largely replaced the older oblique illumination (OI) technique, which was available on reflected light microscopes prior to about 1975. In OI, the vertical illuminator is offset from perpendicular, producing shading effects that reveal height differences. This procedure reduces resolution and yields uneven illumination across the field of view. Nevertheless, OI was useful when people needed to know if a second phase particle was standing above or was recessed below the plane-of-polish, and is still available on a few microscopes. OI can be created on any microscope by placing a piece of paper under one corner of the mount so that the plane-of-polish is no longer perpendicular to the optical axis.
If a specimen must be observed at higher magnification, it can be examined with a scanning electron microscope (SEM), or a transmission electron microscope (TEM). When equipped with an energy dispersive spectrometer (EDS), the chemical composition of the microstructural features can be determined. The ability to detect low-atomic number elements, such as carbon, oxygen, and nitrogen, depends upon the nature of the detector used. But, quantification of these elements by EDS is difficult and their minimum detectable limits are higher than when a wavelength-dispersive spectrometer (WDS) is used. But quantification of composition by EDS has improved greatly over time. The WDS system has historically had better sensitivity (ability to detect low amounts of an element) and ability to detect low-atomic weight elements, as well as better quantification of compositions, compared to EDS, but it was slower to use. Again, in recent years, the speed required to perform WDS analysis has improved substantially. Historically, EDS was used with the SEM while WDS was used with the electron microprobe analyzer (EMPA). Today, EDS and WDS is used with both the SEM and the EMPA. However, a dedicated EMPA is not as common as an SEM.
Characterization of microstructures has also been performed using x-ray diffraction (XRD) techniques for many years. XRD can be used to determine the percentages of various phases present in a specimen if they have different crystal structures. For example, the amount of retained austenite in a hardened steel is best measured using XRD (ASTM E 975). If a particular phase can be chemically extracted from a bulk specimen, it can be identified using XRD based on the crystal structure and lattice dimensions. This work can be complemented by EDS and/or WDS analysis where the chemical composition is quantified. But EDS and WDS are difficult to apply to particles less than 2-3 micrometers in diameter. For smaller particles, diffraction techniques can be performed using the TEM for identification and EDS can be performed on small particles if they are extracted from the matrix using replication methods to avoid detection of the matrix along with the precipitate.
A number of techniques exist to quantitatively analyze metallographic specimens. These techniques are valuable in the research and production of all metals and alloys and non-metallic or composite materials.
Microstructural quantification is performed on a prepared, two-dimensional plane through the three-dimensional part or component. Measurements may involve simple metrology techniques, e.g., the measurement of the thickness of a surface coating, or the apparent diameter of a discrete second-phase particle, (for example, spheroidal graphite in ductile iron). Measurement may also require application of stereology to assess matrix and second-phase structures. Stereology is the field of taking 0-, 1- or 2-dimensional measurements on the two-dimensional sectioning plane and estimating the amount, size, shape or distribution of the microstructure in three dimensions. These measurements may be made using manual procedures with the aid of templates overlaying the microstructure, or with automated image analyzers. In all cases, adequate sampling must be made to obtain a proper statistical basis for the measurement. Efforts to eliminate bias are required.
Some of the most basic measurements include determination of the volume fraction of a phase or constituent, measurement of the grain size in polycrystalline metals and alloys, measurement of the size and size distribution of particles, assessment of the shape of particles, and spacing between particles.
Standards organizations, including ASTM International's Committee E-4 on Metallography and some other national and international organizations, have developed standard test methods describing how to characterize microstructures quantitatively.
For example, the amount of a phase or constituent, that is, its volume fraction, is defined in ASTM E 562; manual grain size measurements are described in ASTM E 112 (equiaxed grain structures with a single size distribution) and E 1182 (specimens with a bi-modal grain size distribution); while ASTM E 1382 describes how any grain size type or condition can be measured using image analysis methods. Characterization of nonmetallic inclusions using standard charts is described in ASTM E 45 (historically, E 45 covered only manual chart methods and an image analysis method for making such chart measurements was described in ASTM E 1122. The image analysis methods are currently being incorporated into E 45). A stereological method for characterizing discrete second-phase particles, such as nonmetallic inclusions, carbides, graphite, etc., is presented in ASTM E 1245.
An electron microscope is a microscope that uses a beam of electrons as a source of illumination. They use electron optics that are analogous to the glass lenses of an optical light microscope to control the electron beam, for instance focusing them to produce magnified images or electron diffraction patterns. As the wavelength of an electron can be up to 100,000 times smaller than that of visible light, electron microscopes have a much higher resolution of about 0.1 nm, which compares to about 200 nm for light microscopes. Electron microscope may refer to:
Microscopy is the technical field of using microscopes to view objects and areas of objects that cannot be seen with the naked eye. There are three well-known branches of microscopy: optical, electron, and scanning probe microscopy, along with the emerging field of X-ray microscopy.
A microscope is a laboratory instrument used to examine objects that are too small to be seen by the naked eye. Microscopy is the science of investigating small objects and structures using a microscope. Microscopic means being invisible to the eye unless aided by a microscope.
A scanning electron microscope (SEM) is a type of electron microscope that produces images of a sample by scanning the surface with a focused beam of electrons. The electrons interact with atoms in the sample, producing various signals that contain information about the surface topography and composition of the sample. The electron beam is scanned in a raster scan pattern, and the position of the beam is combined with the intensity of the detected signal to produce an image. In the most common SEM mode, secondary electrons emitted by atoms excited by the electron beam are detected using a secondary electron detector. The number of secondary electrons that can be detected, and thus the signal intensity, depends, among other things, on specimen topography. Some SEMs can achieve resolutions better than 1 nanometer.
The optical microscope, also referred to as a light microscope, is a type of microscope that commonly uses visible light and a system of lenses to generate magnified images of small objects. Optical microscopes are the oldest design of microscope and were possibly invented in their present compound form in the 17th century. Basic optical microscopes can be very simple, although many complex designs aim to improve resolution and sample contrast.
Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through a specimen to form an image. The specimen is most often an ultrathin section less than 100 nm thick or a suspension on a grid. An image is formed from the interaction of the electrons with the sample as the beam is transmitted through the specimen. The image is then magnified and focused onto an imaging device, such as a fluorescent screen, a layer of photographic film, or a sensor such as a scintillator attached to a charge-coupled device.
A microscope slide is a thin flat piece of glass, typically 75 by 26 mm and about 1 mm thick, used to hold objects for examination under a microscope. Typically the object is mounted (secured) on the slide, and then both are inserted together in the microscope for viewing. This arrangement allows several slide-mounted objects to be quickly inserted and removed from the microscope, labeled, transported, and stored in appropriate slide cases or folders etc.
Electropolishing, also known as electrochemical polishing, anodic polishing, or electrolytic polishing, is an electrochemical process that removes material from a metallic workpiece, reducing the surface roughness by levelling micro-peaks and valleys, improving the surface finish. Electropolishing is often compared to, but distinctly different from, electrochemical machining. It is used to polish, passivate, and deburr metal parts. It is often described as the reverse of electroplating. It may be used in lieu of abrasive fine polishing in microstructural preparation.
Energy-dispersive X-ray spectroscopy, sometimes called energy dispersive X-ray analysis or energy dispersive X-ray microanalysis (EDXMA), is an analytical technique used for the elemental analysis or chemical characterization of a sample. It relies on an interaction of some source of X-ray excitation and a sample. Its characterization capabilities are due in large part to the fundamental principle that each element has a unique atomic structure allowing a unique set of peaks on its electromagnetic emission spectrum. The peak positions are predicted by the Moseley's law with accuracy much better than experimental resolution of a typical EDX instrument.
Electron backscatter diffraction (EBSD) is a scanning electron microscopy (SEM) technique used to study the crystallographic structure of materials. EBSD is carried out in a scanning electron microscope equipped with an EBSD detector comprising at least a phosphorescent screen, a compact lens and a low-light camera. In this configuration, the SEM incident beam hits the tilted sample. As backscattered electrons leave the sample, they interact with the crystal's periodic atomic lattice planes and diffract according to Bragg's law at various scattering angles before reaching the phosphor screen forming Kikuchi patterns (EBSPs). EBSD spatial resolution depends on many factors, including the nature of the material under study and the sample preparation. Thus, EBSPs can be indexed to provide information about the material's grain structure, grain orientation, and phase at the micro-scale. EBSD is applied for impurities and defect studies, plastic deformation, and statistical analysis for average misorientation, grain size, and crystallographic texture. EBSD can also be combined with energy-dispersive X-ray spectroscopy (EDS), cathodoluminescence (CL), and wavelength-dispersive X-ray spectroscopy (WDS) for advanced phase identification and materials discovery.
Failure analysis is the process of collecting and analyzing data to determine the cause of a failure, often with the goal of determining corrective actions or liability. According to Bloch and Geitner, ”machinery failures reveal a reaction chain of cause and effect… usually a deficiency commonly referred to as the symptom…”. Failure analysis can save money, lives, and resources if done correctly and acted upon. It is an important discipline in many branches of manufacturing industry, such as the electronics industry, where it is a vital tool used in the development of new products and for the improvement of existing products. The failure analysis process relies on collecting failed components for subsequent examination of the cause or causes of failure using a wide array of methods, especially microscopy and spectroscopy. Nondestructive testing (NDT) methods are valuable because the failed products are unaffected by analysis, so inspection sometimes starts using these methods.
Focused ion beam, also known as FIB, is a technique used particularly in the semiconductor industry, materials science and increasingly in the biological field for site-specific analysis, deposition, and ablation of materials. A FIB setup is a scientific instrument that resembles a scanning electron microscope (SEM). However, while the SEM uses a focused beam of electrons to image the sample in the chamber, a FIB setup uses a focused beam of ions instead. FIB can also be incorporated in a system with both electron and ion beam columns, allowing the same feature to be investigated using either of the beams. FIB should not be confused with using a beam of focused ions for direct write lithography. These are generally quite different systems where the material is modified by other mechanisms.
Characterization, when used in materials science, refers to the broad and general process by which a material's structure and properties are probed and measured. It is a fundamental process in the field of materials science, without which no scientific understanding of engineering materials could be ascertained. The scope of the term often differs; some definitions limit the term's use to techniques which study the microscopic structure and properties of materials, while others use the term to refer to any materials analysis process including macroscopic techniques such as mechanical testing, thermal analysis and density calculation. The scale of the structures observed in materials characterization ranges from angstroms, such as in the imaging of individual atoms and chemical bonds, up to centimeters, such as in the imaging of coarse grain structures in metals.
The environmental scanning electron microscope (ESEM) is a scanning electron microscope (SEM) that allows for the option of collecting electron micrographs of specimens that are wet, uncoated, or both by allowing for a gaseous environment in the specimen chamber. Although there were earlier successes at viewing wet specimens in internal chambers in modified SEMs, the ESEM with its specialized electron detectors and its differential pumping systems, to allow for the transfer of the electron beam from the high vacuum in the gun area to the high pressure attainable in its specimen chamber, make it a complete and unique instrument designed for the purpose of imaging specimens in their natural state. The instrument was designed originally by Gerasimos Danilatos while working at the University of New South Wales.
Replication, in metallography, is the use of thin plastic films to nondestructively duplicate the microstructure of a component. The film is then examined at high magnifications.
Nanometrology is a subfield of metrology, concerned with the science of measurement at the nanoscale level. Nanometrology has a crucial role in order to produce nanomaterials and devices with a high degree of accuracy and reliability in nanomanufacturing.
Immunolabeling is a biochemical process that enables the detection and localization of an antigen to a particular site within a cell, tissue, or organ. Antigens are organic molecules, usually proteins, capable of binding to an antibody. These antigens can be visualized using a combination of antigen-specific antibody as well as a means of detection, called a tag, that is covalently linked to the antibody. If the immunolabeling process is meant to reveal information about a cell or its substructures, the process is called immunocytochemistry. Immunolabeling of larger structures is called immunohistochemistry.
Ceramography is the art and science of preparation, examination and evaluation of ceramic microstructures. Ceramography can be thought of as the metallography of ceramics. The microstructure is the structure level of approximately 0.1 to 100 µm, between the minimum wavelength of visible light and the resolution limit of the naked eye. The microstructure includes most grains, secondary phases, grain boundaries, pores, micro-cracks and hardness microindentations. Most bulk mechanical, optical, thermal, electrical and magnetic properties are significantly affected by the microstructure. The fabrication method and process conditions are generally indicated by the microstructure. The root cause of many ceramic failures is evident in the microstructure. Ceramography is part of the broader field of materialography, which includes all the microscopic techniques of material analysis, such as metallography, petrography and plastography. Ceramography is usually reserved for high-performance ceramics for industrial applications, such as 85–99.9% alumina (Al2O3) in Fig. 1, zirconia (ZrO2), silicon carbide (SiC), silicon nitride (Si3N4), and ceramic-matrix composites. It is seldom used on whiteware ceramics such as sanitaryware, wall tiles and dishware.
Forensic materials engineering, a branch of forensic engineering, focuses on the material evidence from crime or accident scenes, seeking defects in those materials which might explain why an accident occurred, or the source of a specific material to identify a criminal. Many analytical methods used for material identification may be used in investigations, the exact set being determined by the nature of the material in question, be it metal, glass, ceramic, polymer or composite. An important aspect is the analysis of trace evidence such as skid marks on exposed surfaces, where contact between dissimilar materials leaves material traces of one left on the other. Provided the traces can be analysed successfully, then an accident or crime can often be reconstructed. Another aim will be to determine the cause of a broken component using the technique of fractography.
Holger F. Struer was a Danish chemist and founder of "H. Struers Chemiske Laboratorium" in 1875 at Skindergade 38, the centre of Copenhagen. Struers introduced in 1943 Micropol, a new principle for electrolytic polishing which made the preparation process within metallography more controlled in order to achieve better preparation results.