Materials Science Lab Grading Outline

The lab grade for the labs done in Jolley 103 will be broken down as indicated below. Lab Reports 3 x 15% ea. = 45% Attendance = 45% Lab Notebook = 10% There are three series of labs and three experiments in each series that will be run in Jolley 103. The labs that will be performed are listed below: Series I Mechanical Properties of Materials Experiment I Tensile and Flexural Properties of Materials Experiment II Impact and Fatigue Testing Experiment III Hardness Testing Series II The Structure of Materials and Metallography Experiment I Crystal Structure Models Experiment II X-Ray Diffraction Experiment III Microstructures of Metals and Alloys Series III Processing of Materials Experiment I Strain Hardening Experiment II Recrystallization Annealing Experiment III Heat Treatment & Precipitation Hardening A formal write up of each series of experiments performed is expected (one report per series, so three reports total). If you find it easier to write up a lab report for each experiment that is fine as well. All reports must be prepared with a word processor and must be at least 1.5 spaced to make it easier to read. Tables graphs and figures may be hand drawn, but MUST be neat and labeled. This means use a straight edge if a line should be straight. Although points are not given for the following, points will be deducted if the report is difficult to read, not neat, has excessive grammatical errors, or lacks proper citation of values, figures, and equations not experimentally determined or explicitly given. Attendance will be taken every lab, so make sure you find the sign in sheet and sign in. If you miss one lab day and do not make it up, 30% of your possible attendance points will be deducted. If you miss two or more lab days and do not make them up you will receive no points for attendance and you may receive an incomplete as your grade. You are expected to keep a lab notebook where you write down data and observation about each lab you perform. Writing down good notes and observations when you are performing the labs will make the lab reports much easier to do. Your lab notebook does not need to be neat and should only be turned in with your final (Series III) lab report.

Each lab report should be in a format similar to the example report. The grade for each report will be broken up as follows: Introduction (5%) A concise statement of the purpose or objective of the lab series. Equipment (5%) Brief description of the equipment used for all the labs in the series. The experiment that each piece of equipment was used for should be included. Procedure (5%) A general outline of the lab procedure as followed or explained. If explained, write the procedure as if you performed the experiment. Each experiment should have its own procedure. If some parts of an experiments procedure are the same as some parts of another experiment, you may reference the original experiments procedures which are identical. Results (see individual lab for point breakdown) See individual labs for required results. Results must be presented in tabular or graphical form and should be broken up by experiment. Discussion of Results (see individual lab for point breakdown) See individual labs for specific requirements. Discussion points should be clearly labeled and this section should be broken up by experiment. Conclusions (5%) Statements of fact which are related directly to the purpose of the series of experiments and the results from the experiments. These facts can be bulleted rather than presented in paragraph form. Appendix (5%) Include sample calculations and anything else relevant to the report not included in other sections. The due dates for the lab reports are as follows:
Series I Series II Series III June 25 July 11 July 30

The lab reports are due by the end of the day, and can be turned in to Brian Fillenwarth's pendaflex. Labs will be penalized 4% per day they are late. If a lab is more than 1 week late, it will not be graded and you will receive no points for it. If you need to turn a lab in over the weekend, you may email it to Brian Fillenwarth (baf2@cec.wustl.edu), but this is the only situation when you should email your report. You are still expected to turn a hard copy into Brian Fillenwarth's pendaflex the following Monday. If you need to turn your lab report in late notify Brian Fillenwarth when you turn it in, otherwise it will be marked later than it should be.

Series I Experiment I Tensile and Flexural Properties of Materials Background Reading: Section 6.2 6.8, Section 12.9, & Section 15.2 15.3

1. The Tensile Test and Stress-Strain Diagram: The tensile test measures the resistance of a material to a static or slowly applied force. A test set up is shown in Figure 1.1.1. Sheet/plate and round specimens conforming to ASTM (American Society for Testing of Materials) specifications are used for the measurement of tensile properties. The specimen is gripped between the grips shown and a force F is applied by moving one of the crossheads. The strain rates are very small (10 -4/s to 10-2/s). The force acting on the specimen is measured with a load cell mounted on the machine. A strain gauge or extensometer is used to measure the amount that the specimen elongates between the gauge marks when the force is applied. From the load and elongation values, stress ( ) acting on the specimen and strain ( ) undergone by the specimen are calculated using Equation 1.1.1 and Equation 1.1.2.

/ Ao / Lo

Equation 1.1.1 Equation 1.1.2

In these equations Ao is the initial cross sectional area, Lo is the initial length of the specimen, and is the elongation at any instant. From the stress-strain values, a stress-strain curve is plotted. The stress-strain curve of an aluminum alloy is shown in Figure 1.1.2 and the important properties determined from the stress-strain curves are indicated on the diagram.

Figure 1.1.1 Schematic of a tensile test set up (from Callister)

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Figure 1.1.2 Stress-strain curve of an aluminum alloy from a tensile test (from Askeland and Phule) 2. Experiment: You will be given one plate 6061-T6 aluminum tensile specimen and two plate polytetrafluoroethylene (Teflon) tensile specimens. You will perform tensile tests on the above samples aluminum at a strain rate of 1 x 10-3/s and the Teflon at strain rates of 5 x 10-2/s and 5 x 10-3/s. Obtain stress-strain curves at different strain rates, determine the salient mechanical properties, discuss the deformation characteristics of the two types of materials, and draw conclusions about the data obtained for the two types of materials. 3. Procedure: 1. Measure and tabulate the gauge length, gauge width, and gauge thickness of the specimens. Calculate and record the cross sectional area of each specimen. 2. Determine the crosshead speeds corresponding to the strain rates.

Crosshead speed [ in/min ]= strain rate [1/sec ] x gauge length [ in ] x 60 [sec/min ] Equation 1.1.3
3. Set machine ranges. For aluminum: 20% load, 0.2 in. displacement. For Teflon: 10% load, 10 in. displacement. 4. Grip the specimen in the grips making sure there is no significant load on the sample. Also make sure the grips are secured tight to prevent the specimen from slipping during loading. 5. Start the test and the data acquisition software at the same time, and stop both when the specimen fractures. 4. The Flexure Test: In many brittle materials, such as ceramics, the normal tensile test cannot easily be performed because of the presence of flaws at the surface, difficulty of preparing test specimens and

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premature fracture during gripping of the samples for tensile testing. Such materials may be tested using the flexure test shown in Figure 1.1.3.

Figure 1.1.3 Schematic of a flexure test set up (from Callister) By applying the load at three points and causing bending, a tensile force acts on the material opposite the midpoint and initiates fracture at this location. By knowing the load ( F ), the flexural stress ( f ) can be calculated using Equation 1.1.4 or Equation 1.1.5. The flexural strength of a material is simply the maximum flexural stress sustained by the test specimen. Rectangular specimen: Cylindrical specimen:

3F L 2 b d2 F L f= R3
f=

Equation 1.1.4 Equation 1.1.5

The variables in these equations are defined as shown in Figure 1.1.3. During bending, a specimen is subjected to both compressive and tensile stresses so the magnitude of its flexure strength is greater than its tensile strength. By knowing the deflection of the specimen ( D ), the flexural strain ( f ) can be determined using Equation 1.1.6.
f=

6D d L2

Equation 1.1.6

In this equation, d represents the specimen depth and L represents the span length. 5. Experiment: Using the ceramic rod provided, you will perform a three point bend test on the MTS machine in the laboratory. You will obtain a load deflection plot and will need to compute the flexure strength of the sample. 6. Procedure: 1. Measure and tabulate the diameter of the rod and the distance between the supports. 2. Place the specimen in the machine and preload the specimen to 10 lbs [TA will perform this step]. 3. Input specimen data into computer and start test using a crosshead speed of 0.01 in/min. 7. Results: 1. Stress-strain curves for all tensile specimens and the flexural specimen. (4%)

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2. Table comparing experimental and book/online values of yield strength, tensile strength, modulus of elasticity, and percent elongation for the tensile specimens. (4%) 9. Discussion of Results: 1. Describe the aluminum stress-strain curve. What are the different stages? When do they occur? Why do they occur? (3%) 2. Compare the two Teflon samples. Does experimental error adequately explain the differences? What are other possible explanations for the differences? (3%) 3. Compare the slow strain rate Teflon sample to the aluminum sample. Are there any additional stages in this stress-strain curve or any stages missing? If so, why is this? (3%) 4. Describe any differences between experimental and book/online values for the tensile and flexural tests. Note the flexural strength provided by the manufacturer of the flexure sample is 54 ksi. Are the book/online values for the tensile and flexural tests in good agreement? If not, what are possible reasons for the discrepancies? (3%) 5. Discuss the behavior of brittle materials in relation to ductile behavior of metals and alloys and explain some of the factors responsible for brittle fracture of ceramics. (2%) 6. Comment on the dependence of flexure strength on specimen size and the variability in the measured strengths of brittle materials. (3%)

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Series I Experiment II Impact and Fatigue Testing Background Reading: Chapter 8

1. The Impact Test: The impact test is used primarily to distinguish between ductile and brittle behavior of materials under conditions of impact loading. Two standardized tests, the Charpy and Izod tests shown schematically in Figure 1.2.1, are used. The two tests differ only in the notch dimensions and orientation of the notch relative to direction of the hammer blow. The notched bar is placed in a fixed support, and a wedge shaped hammer of known mass (and potential energy) is allowed to fracture the bar. The energy absorbed in the fracture is read on a scale calibrated in ft-lbs.

Figure 1.2.1

A drawing of an impact testing machine and sample orientations (from Callister)

2. Experiment: Four 1018 cold drawn steel samples and two polymeric (Lexan and Plexiglass) samples will be provided. Using the Charpy testing apparatus, you will be required to perform impact tests on steel samples at four different temperatures: submerged in liquid nitrogen (about -200oC), frozen (about 0oC), room temperature (about 20oC), and furnace heated (to about 200oC). Steels tend to

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behave in a brittle fashion over certain temperature ranges, and undergo what is known as a ductile to brittle transition with increasing test temperature. This ductile-brittle transition temperature (DBTT) can be detected by the change in impact strength as measured in the test and can also be observed in the change in the appearance of the fracture surface of the samples tested at different temperatures. Using the Izod testing apparatus, determine the impact energies of the two polymeric samples. 3. Procedure: 1. Place one steel sample in the oven (record the actual temperature and verify it is close to 200oC), one steel sample in the freezer, and one steel sample in the liquid nitrogen. 2. Get a calibration value for the impact tester. 3. Run impact tests for all four steel samples. Make sure to wait at least 5 minutes before testing the freezer, oven, and liquid nitrogen samples to let them get to their test temperatures. 4. Repeat steps 2 and 3 for the polymeric samples. 4. The Fatigue Test: The response of a material to cyclic loading conditions is determined from stress-amplitude controlled and strain-amplitude controlled fatigue tests. A schematic diagram of a rotatingbending test apparatus, commonly used for testing, is shown in Figure 1.2.2. Compression and tensile stresses are imposed on the specimen as it is simultaneously bent and rotated. Tests are performed at different stress amplitudes (S) and the number of cycles to failure (N) is recorded. S-N curves can be constructed from this data. From this, fatigue limit/endurance limit and fatigue lives are determined.

Figure 1.2.2 Schematic of a rotating-bending fatigue test machine (from Callister) 5. Experiment: The instructor will demonstrate the operation of a rotating-bending fatigue test machine. S-N data for a ferrous (cast iron) and a non-ferrous (brass) sample is provided in Table 1.2.1 and 1.2.2.
Table 1.2.1 - Cast Iron Data Stress Amplitude (MPa) Cycles to Failure 248 1E+05 236 3E+05 224 1E+06 213 3E+06 201 1E+07 193 3E+07 193 1E+08 193 3E+08

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Table 1.2.2 - Brass Data Stress Amplitude (MPa) Cycles to Failure 310 2E+05 223 1E+06 191 3E+06 168 1E+07 153 3E+07 143 1E+08 134 3E+08 127 1E+09

6. Results: 1. 2. 3. 4.

Table with impact energies for steel and polymer samples. (2%) Impact energy vs. temperature curve for steel. (2%) Approximate steel DBTT from experimental data (clearly indicate on curve). (1%) S-N plots for cast iron and brass. (5%)

7. Discussion of Results: 1. Discuss the appearance of the steel fracture surfaces and polymer fracture surfaces. How did the surface appearance change at different temperatures (for steel)? Why is this and what does it mean? (3%) 2. Were the relative impact energies as expected for the different temperature steel samples? If so, why do the impact energies behave in this way? If not, what was expected and why? (4%) 3. Is the experimental DBTT close to a book/online DBTT value (note that 1018 steel has 0.18 wt% carbon)? How was the DBTT determined? Why is the DBTT important? (2%) 4. Compare the steel impact energies to polymer impact energies and compare the two polymer impact energies. (1%) 5. Discuss the cast iron and brass S-N curves. Can anything be concluded from these curves? If so, what and how? (6%)

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Series I Experiment III Hardness Testing Background Reading: Section 6.10 6.11
1. The Hardness Test: give a measure of the ductility of the material as well as its strength. Hardness testing is also used on heat treated steels to determine depth of decarburization of a steel surface after heat treatment. The main advantages of hardness tests are: 1. They are simple and inexpensive 2. They are nondestructive In a typical hardness test, an indentation is made on the surface of a sample by the application of a load, and depth and dimensions of the indentation are measured. The ratios of applied loads and indentation dimensions are expressed as hardness numbers. The most commonly used hardness testing methods are summarized in Table 1.3.1. The load and indenter size/type associated with all of the Rockwell and Superficial Rockwell scales are summarized in Table 1.3.2 and 1.3.3. Table 1.3.1 Hardness Testing Methods (from Callister)

Table 1.3.2 Rockwell Scales (from Callister)

Table 1.3.3

Superficial Rockwell Scales (from Callister)

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2. Experiment: Determine, using suitable hardness testing methods and suitable scales, the hardness numbers of C11000-H04 copper, 6061-T6 aluminum, 1018 cold drawn steel, and Inconel 718 AMS 5596 samples. 3. Procedure: Rockwell: 1. Verify the tester is on the correct scale and has the correct indenter and load (HRF for copper and aluminum, HRB for steel, and HRA for Inconel). 2. Test each sample 3 times making sure each test site is not near an edge or another test site (at least 3 indention diameters away). Vickers: 1. Verify the tester has been zeroed. 2. Prepare a sample for evaluation. 3. Focus the sample and center on an area with no other test sites or edges within 3 indention diameter. 4. Switch to the indenter, indent sample, and switch back to the microscope. 5. Measure the width and height of indention to get the hardness value. Test each sample 3 times. 4. Results: 1. Table of all hardness values, the mean, the standard deviation, and the coefficient of variation (standard deviation/mean). (4%) 2. Table directly comparing hardness values of the two testers (convert Rockwell to Vickers or Vickers to Rockwell to compare). (3%) 3. Table of tensile strengths corresponding to each samples hardness number. (3%) 5. Discussion of Results: 1. How does the coefficient of variation of the two test methods compare? What might explain the difference if there is one? (5%) 2. Do both sets of data (Vickers and Rockwell) give similar hardness values when converted? Discuss any trend in the differences as well as reasons which might explain any differences. (6%) 3. Table comparing experimental tensile strengths to book/online values. Indicate the percent error. If the results are far off, discuss possible reason for this. (3%) 6. Useful Information: 1. All Rockwell to Vickers conversions can be found here: http://www.grantadesign.com/resources/materials/hardnesscharts.htm 2. Figure 6.19 in your text can be used to determine an approximate tensile strength for all specimens except aluminum.

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determine the copper specimen tensile stress. Extrapolation of the curve may be necessary and is acceptable in this case.

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Series II The Structure of Materials and Metallography

Properties of all types of materials arise from their structure, from the manner in which their constituent atoms aggregate into hierarchies of molecular or crystalline order or into disordered amorphous structures. Most of the properties observed and exploited in materials are cooperative properties of the aggregates rather than of the constituent atoms and simple molecules. Therefore, structure is of interest at various levels. For example, certain properties may be explained atomistically in terms of the crystal structure (defect structure), while many properties relate to either the microstructure or macrostructure of the material. The second series of experiments deals with some aspects of the structure at each of these levels. Note that if individual reports are being written for each lab, only the Results section is needed for the Crystal Structure Models lab (just answer the questions in Sections 3 and 4 in the handout, no intro, etc. needed).

Series II Experiment I Crystal Structure Models Background Reading: Section 3.2 Section 3.12
1. Crystal Structure Models: Hard sphere models will be studied to understand various aspects of atomic arrangement in crystalline materials. 2. Experiment: This experiment demonstrates the atom packing arrangements in perfect crystals. 3. Procedure & Discussion: 1. From looking at the crystal structure model, determine the close-packed planes in the hexagonal close packed (HCP) structure. Note that the HCP structure is formed by the ABAB close-packed planes. Write down the family of planes in proper Miller-Bravais format. (3%) 2. From looking at the crystal structure model, determine the close-packed planes in the face centered cubic (FCC) structure. Note that the FCC structure is formed by the ABCABC close-packed planes and is sitting diagonally. Write down the family of planes in proper Miller format. (3%) 3. From looking at the FCC structure, choose one close-packed plane and determine the direction normal to it. Write down the close packed plane and the direction in proper crystallographic notation. What does this tell you about the orientation of the FCC unit cell with respect to the layers of close packed planes? (2%) 4. Sketch a tetrahedral void and the atoms surrounding it. (1%) 5. Sketch an octahedral void and the atoms surrounding it. (1%) 6. Locate the positions of the octahedral and tetrahedral voids in the FCC structure. Describe where they are. Determine the total number of each type of void in a FCC unit cell (note that fractions of a void count towards the total). (4%) 7. From looking normal to the close packed planes in the FCC structure, determine if the octahedral or tetrahedral voids can be seen through when two close-packed planes are superimposed. (1.5%) 8. From looking normal to the close packed planes in the FCC structure, determine if the octahedral or tetrahedral voids can be seen through when three close-packed planes are superimposed. (1.5%) 4. After Lab: 1. Compute the planar packing fraction of (100), (110), and (111) planes in FCC and BCC unit cells. Note the planar packing fraction is the area of the atoms centered on the plane divided by the area of the plane. Your answers should be a percentage and will not contain R. Show ALL work. (4%) 2. Calculate the radius of both the octahedral and tetrahedral voids (interstices) relative to the radius of the atoms. Show ALL work. Why is this important? (4%) Hints: 1. The octahedral void will be in the same plane as some of the coordinate atoms. 2. The tetrahedral void can be modeled in a cube by placing spheres on some corners to represent the coordinate atoms which surround the void (see Figure 2.1.1). Note that the spheres are close-packed along the diagonals (AH, CH, AC, AF, CF, and FH) in Figure 2.1.1. By knowing that the void is at the center of this cube, the void radius can be found by determining the distance of one diagonal of the cube to the opposite diagonal (BH).

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This distance is equal to 2R+2r where R is the radius of the atoms and r is the radius of the void.

B
Figure 2.1.1 Cube Containing Tetrahedral Void

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Series II Experiment II X-Ray Diffraction Background Reading: Section 3.16

1. X-Ray Diffraction: Much of our understanding regarding the atomic and molecular arrangements in solids has resulted from x-ray diffraction investigations. Diffraction occurs when a wave encounters a series of regularly spaced obstacles, that: 1. Are capable of scattering the wave 2.

magnitude to the wavelength

When an x-ray beam encounters electrons, it is scattered in all directions. When x-rays are scattered by the atomic electrons in a regular crystal, however, the scattered beams will have measurable intensities only in certain definite directions. This is because the scattered beams in general are out of phase with one another and so interfere destructively. When the scattered rays are in phase with one another they interfere constructively, and this process is called x-ray diffraction. The conditions necessary for x-ray diffraction are expressed mathematically in

2 d sin ( )

Equation 2.2.1

In this equation, is the angle between the incident x-ray beam and a reflecting (diffracting) plane in the crystal, d is the interplanar spacing, is the wavelength of the x-rays, and the n , is the number of wavelengths in the path difference between x-rays order of reflection, diffracted by adjacent parallel planes. As n increases the intensity of a reflection decreases, so one normally encounters only first and second order reflections (for this lab n= 1 ).

conditions for diffraction from either: 1. Adjacent atoms in one plane or 2. Atoms in adjacent parallel planes are the same. This condition is realized only for certain discrete values of the angle. Such discrete values are called Bragg angles. The magnitude of the distance between two adjacent and parallel planes, d , is a function of the Miller indices as well as lattice parameters. For cubic crystals:

d hkl =

a h +k 2 +l 2
2

Equation 2.2.2

in which a is the lattice parameter. Using Equation 2.2.1 and Equation 2.2.2, and knowing the conditions for diffraction in different crystal structures, it is possible to: 1. Identify the crystal structure of a specimen

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2. Determine the lattice parameters The Debye Scherrer Powder Method and Diffractometer Method are the most commonly used methods for x-ray diffraction studies. In a typical x-ray diffractometer, a specimen, S , in the form of a flat plate is supported so that rotations about the axis labeled O are possible (see Figure 2.2.1). This axis is perpendicular to the plane of the page. The monochromatic x-ray beam is generated at point T and the intensities of diffracted beams are detected with a counter labeled C as shown in Figure 2.2.1. As the counter moves at constant angular velocity, a recorder automatically plots the diffracted beam intensity (monitored by the counter) as a function of . Angles at which intensity peaks are observed are the Bragg angles. Thus by experimentally measuring Bragg angles, crystal structure analysis and specimen identification can be carried out.

Figure 2.2.1 Schematic of X-Ray Diffractometer 2. Experiment: You will be obtaining an X-ray diffraction scan of a copper specimen (face centered cubic structure) and comparing it to the diffraction scan in Figure 2.2.2. You will also receive a diffraction scan of an unknown specimen and will be required to identify it using books which will be provided in the lab. 3. Procedure: X-Ray Diffraction Procedure will be explained in lab Specimen Identification: 1. Determine the order of the samples peaks from highest intensity to lowest. 2. Compute the interplanar spacing, d , using Equation 2.2.1. Note the wavelength, , is 1.54 . 3. Find the material that most closely matches all the interplanar spacing values in the book provided. Note that the book interplanar spacing values are in ngstrm, and they are listed with the highest intensity peak first.

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4. Results: 1. Compute the lattice parameter of the copper specimen shown in Figure 2.2.2 using Equation 2.2.1 and Equation 2.2.2. Note the wavelength, , is 1.54 , and the angles in the Figure are 2 . (5%) 2. A table containing calculated interplanar spacing values, book interplanar spacing values, and the percent error of these values for the unknown sample. (5%) 5. Discussion of Results: 1. Discuss any differences between the X-ray diffraction scan for the copper specimen shown in the lab, and the scan provided in this packet. (2%) 2. Did any difficulties arise when identifying the unknown sample? What may have caused these difficulties if there were any? What does this indicate about this particular test? (4%) 3. Discuss the advantages and disadvantages to using X-ray diffraction for material classification. (4%) 4. Compute the theoretical density of copper using the lattice parameter previously determined. Compare this with the density of copper found in literature. What might explain any differences in the calculated vs. book values for the density? Is X-ray diffraction a good way to determine the density of a material? What are some other ways that could be used to do this? (5%)

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Series II Experiment III Microstructures of Metals and Alloys Background Reading: Section 4.9 Section 4.11
1. Microstructures of Metals and Alloys: A polycrystalline material consists of an aggregate of many grains, each of which is itself a single crystal. The grains are bounded by grain boundaries, and in general the orientation relations between the various grains are entirely random. For a complete description of a piece of polycrystalline material one needs to know both the crystal structure of the grains and their distribution in the sample being considered. The microscopic study of the grain structure of metals is known as metallography and is carried out by using reflected light. 2. Experiment: You will learn how materials are prepared for examination under the optical microscope. You will examine images of copper, titanium, and steel which were taken under an optical microscope (images will be sent to you). 3. Procedure (will not be performed in lab): 1. A small specimen is embedded in a thermosetting plastic mount. 2. This specimen is then polished successively on different grades of abrasive paper to remove scratches to a fine grade. Final polishing of the sample is done by rubbing it on a soft moist velvet cloth with a polishing past, e.g. fine alumina, magnesia, or diamond dust. 3. The sample is then etched with a suitable chemical reagent solution. When a sample is etched, grain boundaries are attacked which form grooves that are seen as networks of lines as shown in Figure 2.3.1b. Under long term etching, grains themselves are also attacked, forming crystallographic terraces as in Figure 2.3.1c. These reflect the light in various directions, according to their orientation, and so some appear dark and others bright in the image. 4. This prepared surface is viewed in a microscope with reflected light as shown in Figure 2.3.1a. 4. Results: 1. Compute the grain size of the steel specimen using the ASTM grain size method and the linear intercept method. Note this sample is at a magnification of 200x. Use Table 2.3.1 to help convert measured quantities into an ASTM grain size number. Compare these two methods. (6%) 5. Discussion of Results: 1. Discuss the problems associated with determining the grain size of a specimen from a crosssection of that specimen. Can you think of a more accurate way to determine the grain size of a specimen? (5%) 2. Explain why the steel samples grains are two different colors while the other samples are essentially all the same. (5%) 3. Discuss any differences you see in the various heat treatments of the samples. What is a possible explanation for these differences? How does heat treatment affect grain size? (4%) 4. Explain why etching a sample is important to do prior to viewing it under an optical microscope. (5%)

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Series III Processing of Materials

The third series of experiments introduces the students to how processing affects the properties of materials. Deformation processing, recrystallization annealing, heat treatment, and precipitation hardening are used to illustrate the important processing effects. Note that an appendix is not needed for the report on this series of labs and therefore is not worth any points.

Series III Experiment I Strain Hardening

1. Strain Hardening: Metals and alloys can be hardened and strengthened by strain hardening, a process of plastic deformation carried out below the recrystallization temperature of the metal or alloy. A commercially pure copper bar will be furnished to each group, and by the use of a mechanical roller, the bar will be reduced in cross-section in a number of passes of the bar through the rolls. 2. Experiment: In this experiment you will roll a C11000-H04 copper bar to approximately 10%, 20%, 40%, 60%, and 80% reduction in area, and obtain hardness values of the sample at these reductions. You will also look at the microstructure of the specimen at various percent reductions. 3. Procedure: 1. Measure the original cross-sectional area, A o , of the copper bar. 2. Obtain the hardness of the specimen using the Rockwell F scale. Test the sample 3 times and make sure the area being tested is flat. 3. Use the roller to reduce the cross sectional area of the bar. Reduce it by only a small amount. 4. Measure the cross-sectional area, A , of the reduced copper bar and calculate the percent reduction using Equation 3.1.1. A A %R= o Equation 3.1.1 A
o

5. Repeat steps 3 and 4 until a value close to the next one (10%, 20, 40%, 60%, or 80%) is obtained 6. Repeat steps 2 5 until 80% reduction is obtained. 7. At 80% reduction, measure the hardness of the sample using the Rockwell 15-T scale. Test the sample 3 times. 4. Results: 1. Plot a graph showing hardness vs. percent reduction in cross-sectional area. (6%) 2. Plot a graph showing tensile strength vs. percent reduction in cross-sectional area. (2%) 5. Discussion of Results: 1. Discuss the role of dislocations in the strain hardening process. (8%) 2. Discuss the effect of strain hardening on the mechanical properties of metal. (8%) 3. Discuss the changes in the microstructure of the sample as the percent reduction increases. Include images of the sample. (3%)

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Series III Experiment II Recrystallization Annealing

1. Recrystallization Annealing: Cold working is a useful strengthening mechanism. It is also a very effective tool for shaping materials using wire drawing, rolling, extrusion, etc. Cold working leads to effects that are sometime undesirable. Annealing treatments are used to eliminate some or all the effects of cold working. Upon heating of cold worked materials above 0 . 3 T m ( T m is the melting point in K), three processes occur: 1. Recovery 2. Recrystallization 3. Grain Growth During recovery, the tangled dislocations rearrange themselves into low energy configurations called sub (or low angle) boundaries. Such a structure is known as polygonized subgrain structure. During recovery, there is a small decrease in hardness. Microstructural examination reveals an elongated grain structure typical of cold worked materials. Polygonization can best be seen in a transmission electron microscope where one observes 0.2 2 micrometer subgrains. When the cold worked material is heated above a certain temperature called recrystallization temperature, new small grains nucleate at the cell boundaries of the polygonized structure, eliminating most of the dislocations. All the elongated grains are replaced by small equiaxed strain-free grains. This microstructure is called recrystallized grain structure. This can be readily seen by optical microscopic examination. During recrystallization, there is a large decrease in hardness. Following complete crystallization, continued annealing at the same temperature or annealing at higher temperatures results in grain growth coarsening of recrystallized grains, the driving force for such grain growth being a reduction in surface energy (due to reduction in grain boundary area). The grain growth follows Equation 3.2.1

Dt

D o =k t
2

Equation 3.2.1
t

where D o is the initial grain size, and Dt is the grain size after a time

2. Experiment: You will determine the hardness of a brass sample for the conditions shown in Table 3.2.1. 3. Procedure: 1. Verify the tester has been zeroed. 2. Prepare a sample for evaluation. 3. Focus the sample and center on an area with no other test sites or edges within 3 indention diameter. 4. Switch to the indenter, indent sample, and switch back to the microscope. 5. Measure the width and height of indention to get the hardness value. Test each sample 3 times.

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Table 3.2.1 - Brass Test Specimens % Reduction HT Time @ 550 C (min) Recrystallization Testing Group 1 Partially 2 Partially 25 5 Partially 10 Fully 1 Partially 2 Partially Group 1 50 5 Partially 10 Fully 1 Partially 2 Partially Group 2 75 5 Fully 10 Fully 1 Partially 2 Fully Group 3 90 5 Fully 10 Fully o

Hardness Value 83.6, 86.4, 82.7 80.7, 78.4, 79.9 71.5, 71.2, 75.3 64.4, 65.1, 65.5

70.1, 69.1, 69.6

70.4, 72.3, 73.2

69.8, 76.3, 73.8

4. Results 1. Table of hardness values for various conditions. (5%) 5. Discussion of Results 1. Discuss the reasons for the hardness values obtained. Do higher or lower percent cold worked samples in general give higher hardness values? Why is this? What happens as the annealing time increases? Why does this occur? (10%) 2. What is meant by recovery, recrystallization, and grain growth? (5%)

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Series III Experiment III Heat Treatment & Precipitation Hardening

1. Heat Treatment of Steels: There are several heat treatment options available for controlling the microstructures and properties of steels. This lab will examine four of these conditions. 2. Precipitation Hardening: Precipitation hardening is one of the most commonly used strengthening methods in the development of commercial high strength aluminum alloys. The object of precipitation strengthening is to create in a heat-treated alloy, a dense and fine dispersion of precipitated particles in a matrix of deformable metal. The precipitates act as obstacles to dislocation movement and thereby strengthen the heat-treated alloy. The method used for precipitation hardening is identical to that for heat treating steels, but the underlying principles are different. 3. Experiment: Steel: Four samples of 1018 steel will be provided. The four samples have been austenitized at 925 oC for one hour and the following heat treatments have been applied: Annealed: Cooled in the furnace by shutting off the furnace and slowly cooled overnight. Normalized: Sample removed from austenitizing furnace and cooled in still air. Spheroidized: Sample removed from austenitizing furnace and placed in a furnace at 650 o C for seven days. Water quenched: Sample plunged into water and agitated until cooled to room temperature from austenitizing furnace. Hardness tests will be done on all four heat treated samples using the Rockwell B scale. Images of the microstructures of these heat treatments will be analyzed. Aluminum: A commercial 2024 aluminum alloy (4.4% Cu, 1.5% Mg, 0.6% Mn, 93.5% Al) is heat treated to produce a precipitation hardened alloy. The precipitation strengthening process involves the following basic steps: 1. Solution treatment: The alloy is heated to a temperature, T 1 , in the single phase field and soaked at this temperature until a uniform solid solution structure is produced. 2. The alloy is then rapidly quenched to a lower temperature, usually room temperature to retain the high temperature single phase structure as a supersaturated solid solution. 3. The solution treated and quenched alloy is then annealed at some intermediate temperature, T 2 , for different lengths of time to produce uniformly distributed fine precipitates in the matrix. During this aging treatment, the hardness first increases, reaches a peak, and then decreases. This hardness variation results from the change in size, nature, and volume fraction of the precipitates. Hardness tests will be done on Al samples that have been solution treated at T 1 and quenched, as well as solution treated at T 1 and quenched and then heat treated at T 2 for 1, 4, 8, 20, and 48 hours. The Rockwell F scale will be used.

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4. Procedure: Steel: 1. Test the four samples three times each using the Rockwell B scale. Aluminum: 1. Determine the solution treatment temperature, T 1 , and the ideal aging temperature, T 2 , using the book provided. 2. Test the six samples three times each using the Rockwell F scale. 5. Results: 1. A table of hardness values obtained for the steel samples. (4%) 2. A table of hardness values obtained for the aluminum samples. (4%) 3. A hardness vs. aging time plot for aluminum. (4%) 6. Discussion of Results: 1. Discuss the microstructure of the steel samples. What phases are present in each sample? What are the differences between the heat treatments? Include the pictures in your report. (5%) 2. Why do the different phases form in steel? (2%) 3. What are applications for each type of steel? Why is each particular type of steel well suited for those applications? (5%) 4. Why does the hardness first increase and then decrease with the aluminum sample? (4%) 5. Describe the differences between heat treatment of steels and precipitation hardening of aluminum. (5%)

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