TITLE:

INTRODUCTION TO SAMPLE PREPARATION AND OPTICAL MICROSCOPE FOR METALLOGRAPHIC OBSERVATION

ABSTRACT
Verification for make preparation of sample and optical microscope for Metallographic of metal before use it for further experiment. Using several preparatory for standard method of preparation, beginning from a cutting moment, through mounting, grinding, polishing and etching. Standard method of preparation of micro-sections, typically for structure layer was used and microstructure observation, which the surface will get more clearly in optical microscope. Extra attention will be made in Metallographic preparation because the result will effect in damages and deformations of the sample surfaces if the procedure is incorrect.

Table of content

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List of figure List of table Introduction Objective Theory Apparatus Procedure Result Discussion Conclusion Reference Appendix

List of figure

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Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7(a) Figure 7(b)

(Abrasive Cutter) (resins) (Automatic Mounting machine) (Grander Machine) (Polishing Machine) (Ecthing Machine) (Optical Microscope) (Schematic Diagram of Optical Microscope)

Figure 8 Figure 9

(Sand Paper) (Phenolic Powder)

List of table/chart

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INTRODUCTION
Metallographic is the study of the physical structure and components of metals, typically using microscopy. Ceramic and polymeric materials may also be prepared using metallographic techniques, hence the terms ceramography, plastography and, collectively, materialgraphy.

Materials engineers can predict the general behavior of materials by observing their microstructure. Besides the crystallographic nature of a material, imperfections inside a material have an even greater influence on the mechanical properties, example tensile, fatigue, creep, fracture toughness, impact properties. Some defects such as missing planes of atoms, called dislocations, are responsible for plastic deformation of crystalline solids. Others such as grain boundaries, precipitates, twins and cracks alter stress distribution in a material and the accompanying motion of dislocations. Some defects such as missing atoms and dislocations cannot be observed optically except by their effects, such as strain, slip lines. Other defects such as grain boundaries, twins, precipitates, can be observed readily in the microscope. The study of microstructaral details is important due to its correlation with the ensuing mechanical properties of the material. As an example, if material A exhibits a more homogeneous and refined microstructure than material B, it may very well be anticipated that material A will exhibit better room temperature properties when compared to material B.

SAMPLE PREPARATION In the study of metallic materials it is often to analyze the phase exists and grain size in the structure. Details of the structure of metals are not readily visible through naked eyes, but grain structures in metals may be seen with the aid of microscope. Metal characteristics such as grain sizes, effect of heat treatment, and carbon content of steels may be determined by studying the micrograph. For this purpose, the metal that we use in metallurgical examination must prepare and polished carefully before a good microscopic picture can be seen. There is important to ensure that the surface is totally flat and smooth before seeing it under microscope. Any irregularity will appear as a dark surface and will confuse the observer who attempts to analyze a structure. In order to obtain this smooth flat surface, several preparatory steps are required. The following section briefly describe the various steps involved in the metallographic preparation of the samples. a) CUTTING Cutting process is carried out in order to get the desired size of the sample so that it can be easily molded/handle. The type of cutting methods is Abrasive cutter.

FIGURE 1

b) MOLDING Molding process is carried out to make the sample easier to hold throughout the polishing procedure. There are 2 type of mounting 1. COLD MOUNTING 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.

FIGURE 2

2. HOT MOUNTING In hot-mounting the sample is surrounded by an organic polymeric powder which
o

melts under the influence of heat (about 200 C). 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 entrapment 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.

FIGURE 3

c) GRINDING Grinding is done using rotating discs covered with silicon carbide paper and water. There are a number of grades of paper, with 120, 180, 240, 320, 400, 600, 1200, grains of silicon carbide per square inch. 120 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. There are 2 type of grinding.

FIGURE 4 1. ROUGH GRINDING To remove rough scale and gross imperfections on the surface of sample. 2. FINE GRINDING To improve the specimens surface until it begins to shine and reflect light slightly.

d) POLISHING

FIGURE 5

1. ROUGH POLISHING To remove the imperfection that grinding left. 2. FINE POLISHING To remove all starches and leaves a mirror like finish on the surface.

e) ETCHING Etchants are composed of organic or inorganic acid and alkalis dissolved in alcohol, water, or other solvent.Various and alkalis are used to selectively attack the surface of metal to reveal grain boundaries, phases, precipitate, inclusion and variation in composition.

FIGURE 6

INTRODUCTION TO OPTICAL MICROSCOPE When a mirror-like metal surface has been prepared, the structure can be observed under optical microscope for analysis. Before interpreting of the structure that you observe, it is important to understand some of basic operations of optical microscope in metallurgical study. The optical microscope magnifies an image by sending a beam of light through the object as seen in the schematic diagram. The condenser lens focuses the light on the sample and the objective lenses (10X, 40X,, 2000X) magnifies the beam, which contains the image, to the projector lens so the image can be viewed by the observer. In interpreting the microstructure, it is helpful to consult with the phase diagram and to have some knowledge of the composition and thermal history of the specimen. If both resources are used, phase can be often identified and the sequence in which they formed can be traced.

7(a)

7(b)

FIGURE 7

OBJECTIVES
After completing this experiment, students are be able to: Understand the steps required in preparing metallographic sample. Understand the concept of etching and the purpose of this process. Understand the basic function of optical microscope and its operation Use the analysis from the microstructures observed.

THEORY
The grain size of metals are usually expressed as the American Society for Testing and Materials (ASTM) grain size number. The ASTM has prepared 10 standards comparison charts, all having different average grain sizes. To each is assigned a grain size number ,n, ranging from 1 to 10, the larger the number, the smaller the grains. The designation is based on the equation, N = 2n-1. where N is the number of grains in an area of 1 sq. in at 100x magnification. A specimen must be properly prepared to reveal the grain structure, which is photographed at a magnification of 100x. Thus a steel with N=6 has , on average, 32 grains in an area of 1 sq. in. at 100x. Grain size is expressed as the grain size number of the chart that most nearly matches the grains in the micrograph. Straight lines all of the same length are drawn through several photomicrographs that show the grain structure. The grains intersected by each line segment are counted; the line length is then divided by an average of the number of grains intersected, taken over all the line segments. The average grain diameter is found by dividing this result by the linear magnification of the micrographs.

APPARATUS
1. Abrasive cutter 2. Hot Mounting Machine

FIGURE 1

FIGURE 3

3. Grinding Machine

4. Sand Paper

FIGURE 4

FIGURE 8

5. Polishing Machine

6. Ecthing Machine

FIGURE 5

FIGURE 6

7. Optical Microscope

FIGURE 7(a)

8. Phenolic Powder

FIGURE 9

EXPERIMENTAL PROCEDURES
1) Cutting A raw specimen of metal is selected use mild steel. After identifying the type of the raw specimen given, the blade is prepared. It is for higher level of safety, sufficient and the effectiveness of the process. The coolants of the cutter and the machine is ready also safe to use for cutting process. Then the raw specimen is being placed to get as dimension insist in the Abrasive cutter. At the same time safety preparation is in consideration. 2) Molding Use hot molding After cutting finished, then Automatic mounting machine is being checked for ready to use. Time and degree of temperature is being set before molding process is being continued. The phenolic powder is then poured inside to make the mold of the specimen. The process is then waiting for a while until the machine gives alert by its sensor to know the process is success. 3) Grinding With Automatic Grinder Machine After molding process is settled down, the sample which had been mold bring to the Grinder Machine for the next process.

After the machine is checked is ready to use, the roughness sand paper with grade 240 is being chosen to be placed in the machine.

Then the sample is Grind on the sand paper with coolant is on. Variety of sand paper grade is use then based on the roughness stand on the sample from the roughness till the fine sand paper grade.

The step 4 and 5 is repeated again until the crust decrease and disappear.

4) Polishing After grinding session is finished, then Automatic Polishing Machine is being checked for ready to use. Polishing powder or diamond suspension had been mixed with some water is then being put on the surface of polishing place as the machine is not on. After the powder is being placed, then the machine is turn on and polishing process is progress. Polishing process is done with smooth actions to minimize the scratch on the sample. The polishing process is done as the sample is mirror look like.

5) Etching After polishing session is finished, then the sample is bringing through to the etching place. During the etching session, safety guidance is in considered. The sample is then being dropped with some etchant provided by using its tool. After etching the sample, the sample then was being dropped some water on the surface of the sample.

The sample then is being sprayed by air in compressor to remove the balance of water before placing it under microscopic optical.

6) After all the process is done, the sample then being placed under the microscopic optical. 7) All the data are being collect and results is taken down.