ENME 2711

Experiment 5: Metallographic Analysis

Performed: 11/29/2013

Johan Dreher

OBJECTIVE This lab will go through the average experimental procedures for samples that come through the metallographic analysis. These steps, in order, will be: mounting, polishing, etching, photographing, determining the grain size, and ultimately hardness testing. Hardness testing will not be part of this lab. However, hardness testing is a separate experiment, conducted in Experiment 2. Three AISI 1045 steel samples (air, water, and furnace cooled) are considered for the metallographic analysis.

THEORY AND PROCEDURE Mounting Mounting - The mounting operation accomplishes three important functions. First, it protects the specimen edge and maintains the integrity of materials surface features. Second, it fills voids in porous materials. Finally, it improves handling of irregular shaped samples, especially for automated specimen preparation. The majority of metallographic specimen mounting is done by encapsulating the specimen into a compression mounting compound (thermosets phenolics, epoxies, diallyl phthalates or thermoplastics acrylics). Polishing The specimen is polished on the Struers TegraPol-1 using the Struers diamond suspended lubricants. Steel sample polishing consists of five steps. Step one is known as rough polishing. First, the sample is affixed to the Struers Tegra-Pol, and run over #220 grit sandpaper at 300 RPM with 25 N of force and water as lubricant for 1:30 minutes. In the second step, the sample is run over a finer grit polishing pad at 150 RPM with 20 N of force and 9 micrometer diamond lubricant for 2:30 minutes. The third and fourth steps are characterized through finer and finer grit polishing pads at 150 RPM with 25 N of force using a 6 and 3 micrometer diamond lubricant for 3:00 minutes. The fifth step is characterized as final polishing, and includes running the sample over a low nap cloth pad using 0.05 micrometer diamond lubricant at 150 RPM and 20 N of force for 2:00 minutes. After each step, the sample surface should reflect a homogenous surface. Each sample is thoroughly checked between steps. If the sample did not display the required characteristics, then each step is repeated as necessary. Etching The purpose of etching is to optically enhance microstructural features such as grain size and phase features. Etching selectively alters these microstructural features based on composition, stress, or crystal structure. The type of etching used in this laboratory is chemical etching.

Chemical etching selectively attacks specific microstructural features. It generally consists of a mixture of acids or bases with oxidizing or reducing agents. The process of etching the sample occurs after the sample has undergone all the polishing steps. When the sample reflects a smooth homogenous surface, the remaining lubricant is then rinsed off of the surface of the sample and a small amount of etchant is wiped onto its surface. For carbon steels, tin, and nickel alloys the recommended etchant is Nital, which is comprised of 100 ml of Ethanol and between 1/10 ml Nitric acid. This etchant is left on the surface of the sample for anywhere from seconds to minutes. For this steel sample the etchant is left on for approximately 15 seconds. Photographing Photographing will be done on the Shimadzu HMV Hardness Tester. This section of the lab will be done by the students using the steps provided. A lab assistant will be in the lab to assist when necessary. The procedures for photographing samples are: 1. Ensure the Shimadzu HMV is on and that there is no indenter tip in the tester. The indenter tip would be located between the two objective lenses above the sample stage. 2. Locate and double-click CAMS icon on the desktop. (Notice: HMV2 NOTRESPONDING error will appear randomly. Disregard and click OK to continue). 3. Place sample on sample stage and ensure the 10x objective is selected, if not use the lens button on the HMV touchscreen to toggle from 40x to 10x lens. 4. Slowly raise sample stage using lever on the right side of the machine until sample is in focus on the computer screen. 5. Use the two micrometers to navigate the sample and find an appropriate position to take a picture. 6. To take the picture, click SAVE on the bottom left of the CAMS software. 7. Switch to 40x objective lens, find an appropriate area, and take another picture. 8. Lower sample stage and remove specimen. 9. Repeat steps 3-8 for the remaining two samples. 10. Once finished, retrieve photos from lab assistant either by flash drive or email. Determining the Grain Size The grain size is often determined when the properties of the crystalline material are under consideration. In this regard, there exist a number of techniques by which size is specified in terms of average grain volume, diameter, or area. Grain size may be estimated by using an intercept method, described as follows. Straight lines, all the same length, are drawn through several photomicrographs that show the grain structure. The grains intersected by each line segment are counted; the lime 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 photomicrographs. The American Society for Testing and Materials (ASTM) has prepared several standard comparison charts, all having different average grain sizes. To each is assigned a number ranging from 1 to 10, which is termed the grain size number. A specimen must be properly prepared to reveal the grain structure, which is photographed a t a magnification of 100x. Grain size is expressed as the grain size number of the chart that most nearly matches the grains in the micrographs. Thus, a relatively simple and convenient visual determination of grain size number is possible. Grain size number is used extensively in the specification of steels. The rationale behind the assignment of the grain size number to these various charts is as follows. Let n represent the grain size number, and N the average number of grains per square inch at a magnification of 100x. These two parameters are related to each other through the expression: (1) At magnification other than 100x, use of the following modified form of Equation (1) is necessary: ( ) (2)

In this equation, the number of grains per square inch at magnification M. In addition, ) term makes use of the fact that, while magnification is a length the inclusion of the ( parameter, area is expressed in terms of units of length squared. As a consequence, the number of grains per unit area increases with the square of the increase in magnification.

RESULTS AND DISCUSSION 1. Photograph of microstructures of AISI 1045 steel Air cooled 100x

Air cooled 400x

Water cooled 100x:

Water cooled 400x:

Furnace cooled 100x:

Furnace cooled 400x:

CONCLUSIONS

QUESTIONS