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Metallography: Sample Preparation and Examination

Reading Assignment (sections 4.10 and 4.11 in the textbook) Objective The objective of this experiment is to describe metallography and its application to study the microstructure of materials. Students will observe grain boundaries and phases in different metallic samples using an optical microscope. Safety Optical metallography involves the use of etchants (standard solutions containing a variety of chemicals such as strong acids and solvents) which can be very corrosive and poisonous. You must wear gloves and goggles and handle the chemicals with extreme care. You must not have direct skin or eye contact with the etchants. Etchants must be used in well ventilated area. Do not try to smell the etchants. Introduction Our understanding of the behavior of materials depends on our ability to relate properties to microstructures. The microstructure is the geometric arrangement of grains and the different phases present in a material. Grain Boundaries. The first thing we want to learn about any given microstructure is the size and shape of the grains (crystals). Most engineering alloys are polycrystalline (Figure 1). This means that each piece of a metal is made up of a great number of single crystals, or grains, each having a regular crystal structure (for example, FCC, BCC, or HCP). Each grain will have a different crystallographic orientation relative to its neighboring grains. There is a region between adjacent grains where the crystal lattice is disordered due to abrupt change in crystallographic directions. This region is Figure 1: atomic disorder at GB called the grain boundary. The grain size (i.e., the spacing between grain boundaries) greatly influences many properties of a polycrystalline material and thus measuring the grain size in a given microstructure is a routine practice in materials testing. Materials specialists are interested to see the grain boundaries in order to estimate the grain sizes. The average grain size in metals is usually in the order of several to tens of micrometres, which can be measured only by the use of an optical or light microscope (see your text p.82 for description of an optical microscope). An Optical microscope strikes the surface of a specimen with a source of intense light and uses optics to collect the reflected beams of light to form the magnified image. Magnification of optical microscopes can range from 1 to 1000X but 200X is usually sufficient for practical purposes. Contrasts in the reflective image result from differences in reflectivity

of various regions of the microstructure. Photographs taken with optical microscopes (micrographs) play a vital role in our attempts to identify the microstructure of a given material. Second phase particles. Many engineering materials are composed of more than one phase. A phase is defined as a part of material that is distinct from others in crystal structure (BCC, FCC, or HCP) or in composition (Fe is a different phase than Fe3C; and Al is a different phase than Al2O3). Second phase particles having sizes in the range of few micrometers are present in most engineering alloys and are readily observed in an optical microscope. Different phases will appear in micrographs at different gray scale because each reflects light at different intensities depending on its optical properties.



Figure 2: single-phase pure molybdenum showing grain boundaries (250X) (a); malleable cast iron (Fe-C alloy) consists of two phases (200X). Sample Preparation Metallography is the art of preparation of specimens that can be examined by an optical microscope. Examining a metal sample in the microscope without prior preparation will not reveal informative image of the microstructure because roughness and scratches at the surface will reflect the incident light randomly. The preparation starts by cutting a small representative piece of the metal to be studied. The process of sample preparation is schematically summarized in Figure 3.

Figure 3

Mounting. Small samples can be difficult to hold safely during grinding and polishing operations, and their shape may not be suitable for observation on a flat surface. They are therefore mounted inside a polymer block or mount. Cold mounting can be done using two components resins (epoxies) which are liquid to start with but which set solid shortly after mixing. Cold mounting requires very simple equipment consisting of a cylindrical ring which serves as a mould and a flat piece which serves as the base of the mould. The

sample is placed on the flat piece within the mould and the mixture poured in and allowed to set. Cold mounting takes few hours to complete. In hot-mounting the sample is surrounded by an organic polymeric powder which melts under the influence of heat (about 200 oC). Pressure is also applied by a piston, ensuring a high quality mould free of porosity and with intimate contact between the sample and the polymer. This is not the case with cold mounting where the lack of proper contact and the presence of porosity can cause problems such as the entrappment and seepage of etchant during the final stages of preparation. Consequently, hot-mounting should be the preferred way of encapsulating specimens assuming that time and resources permit, and assuming that the heat involved in the process does not influence the sample. Because of time limitation in the lab, specimens have already been mounted for you using hot mounting. Grinding is done using rotating discs covered with silicon carbide paper and water. There are a number of grades of paper, with 180, 240, 400, 1200, grains of silicon carbide per square inch. 180 grade therefore represents the coarsest particles and this is the grade to begin the grinding operation. Always use light pressure applied at the centre of the sample. Continue grinding until all the blemishes have been removed, the sample surface is flat, and all the scratches are in a single orientation. Wash the sample in water and move to the next grade, orienting the scratches from the previous grade normal to the rotation direction. This makes it easy to see when the coarser scratches have all been removed. After the final grinding operation on 1200 paper, wash the sample in water followed by alcohol and dry it before moving to the polishers. Polishing. The polishers consist of rotating discs covered with soft cloth impregnated with a pre-prepared slurry of hard powdery alumina particles (Al2O3, the size ranges from 0.5 to 0.03 m). Begin with the coarse slurry and continue polishing until the grinding scratches have been removed. It is of vital importance that the sample is thoroughly cleaned using soapy water, followed by alcohol, and dried before moving onto the final stage. Any contamination of the final polishing disc will make it impossible to achieve a satisfactory polish. Examining the specimen in the microscope after polishing should reveal mirror like surface. Etching. The purpose of etching is two-fold. Grinding and polishing operations produce a highly deformed, thin layer on the surface which is removed chemically during etching. Secondly, the etchant attacks the surface with preference for those sites with the highest energy, leading to surface relief which allows different crystal orientations, grain boundaries, precipitates, phases and defects to be distinguished in reflected light microscopy as demonstrated in Figure 4. Please adhere to the general safety regulations provided to you at the Figure 4. Surface groove produced by etching and observed in the microscope 3

beginning of this handout. A polished sample is etched using a cotton tip dipped in the etchant. Etching should always be done in stages, beginning with light attack, an examination in the microscope and further etching only if required. If you overetch a sample on the first step then the polishing procedure will have to be repeated. The table below gives the etchants for alloys that will be examined in this experiment.

Sample Al alloys Cu-Zn alloy (brass) Steel and cast irons

Etchant Kellers (2 ml HF +3 ml HCL + 5 ml HNO3+ 190 ml water) 10 ml HNO3+90 ml water Nital (2% HNO3 + 98% ethanol)

Table 1 Common etchants for engineering alloys.

Grain Size Determination When you examine a metallic sample under the microscope, you will notice that there is a distribution of grain sizes. How to report an average grain size? There are many ways to report that but we will consider only the intercept method. Draw few random straight lines through the micrograph. The grain boundaries intersecting each line are counted. The average grain size is obtained by dividing the total length of the lines by the number of intersections taking into account the magnification used to produce the micrograph. Requirements for the report: 1. Each group (2 students each) will grind, polish, and etch one sample and examine the microstructure in the optical microscope. 2. Each group has to report the average grain size, the number of phases present, and provide a sketch of the microstructure. 3. The lab report format should follow your lab instructor.