Heat Treatment & Indentation Hardness Testing

Laboratory 1 and 2 Report

Mechanical Behavior of Engineering Materials (ME108) Fall 2013 University of California at Berkeley

Group 8 Lab Section 104, 1st Rotation

Joey Johnescu Kevin Kung Nhan Lac Nick Renda Jon Saltz

TABLE OF CONTENTS
1.0 2.0 3.0 ABSTRACT ............................................................................................................................ 3 INTRODUCTION .................................................................................................................. 3 THEORY................................................................................................................................. 3
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4.0

EXPERIMENTAL METHODS ............................................................................................ 4

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5.0 6.0 7.0 8.0 9.0 !

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RESULTS ................................................................................................................................ 6 DISCUSSION ......................................................................................................................... 6 CONCLUSIONS..................................................................................................................... 8 REFERENCES ....................................................................................................................... 8 APPENDIX ............................................................................................................................. 9

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1.0

ABSTRACT
In this lab assignment we learned how the microstructure of AISI 1018 and 1045 steels

could by manipulated by heat treatment processes. We were tasked with investigating the effect heat treatment has on the hardness of different steel alloys. Using Rockwell hardness testing machines, we determined that heat treatment roughly doubles a steel samples yield strength. Rapid cooling of high temperature austenitic steel results in a purely martensitic composition, which has much stronger bonds between the iron atoms. We also found that higher carbon content contributes to the strength of a steel alloy, due to the carbon atoms preventing atomic dislocations that occur during plastic deformation. Heat treatment and careful selection of carbon percentage were proven to be effective ways to produce high-strength steel for use in many applications.

2.0

INTRODUCTION
Steel, an alloy of iron and other elements, including carbon, has become a staple in

engineering innovation with applications ranging from railroad tracks to watches; but as engineers continue to push the limits of science, material properties have become the forefront of limitation for mechanical design and manufacturing processes. One such property engineers analyze is the indentation hardness of the material, or the ability of a material to resist plastic deformation due to indentation by a rigid body. Generally, the indentation hardness is measured by pressing a sharp indenter of known geometry and mechanical properties against the test material. Through this lab, students are to learn (1) how the microstructure of materials can be altered by heat treatment followed by rapid cooling (quenching) and (2) how microstructures changes can affect the indentation hardness of materials, testing low-carbon (AISI 1018) and medium-carbon (AISI 1045) steel. For the latter experiment, students will be provided with two calibration blocks and four steel specimens, making three hardness measurements for each sample and recording the results using the Rockwell testing procedure.

3.0
3.1

THEORY
Heat Treatment Metallic alloys vary greatly in their material properties depending on their temperature

history. This behavior is both composition-dependent and time-dependent. A binary alloy with relatively dissimilar components such as carbon steel may be classified as a eutectoid, a hypoeutectoid, or a hypereutectoid depending on the weight ratios of the alloy's components (See Appendix A). In a eutectic alloy, all the components solidify into a single solution at a lower temperature than any other composition. For example, the eutectic composition of carbon steel is 0.76 percent carbon by weight. For a eutectic carbon steel, a laminar ! 3

microstructure known as pearlite is formed immediately upon reaching 748C. A hypoeutectic carbon steel composition has a weight percentage of carbon less than 0.76, and a hypereutectic carbon steel composition has a weight percentage above 0.76. Either !-ferrite or cementite (the components of pearlite) will form first upon cooling, resulting eventually in a mixture of pearlite and either !-ferrite or cementite [1]. The rate of cooling also affects the properties of the material. A Time-Temperature Transformation (TTT) diagram describes the reaction of the material to temperature change against elapsed time (See Appendix B). For carbon steels in general a slow cooling rate allows for the diffusion of carbon atoms, promoting the formation of pearlite. The coarseness of this structure depends on the cooling path taken. If steel is forced to take a very steep cooling path a brittle, needlelike structure known as martensite is formed [2]. Heat treatment is essentially the manipulation of these properties. 3.2 Hardness Hardness is defined as the resistance of a material to deformation from the compressive load of an indenter; this is the basis of the Rockwell hardness test. Hardness testing is important for engineers because it is a useful, easy, and relatively nondestructive way to verify the material properties of manufactured materials. In particular, hardness can be an indicator of the yield strength of the material. As a general rule: !! ! where HV is Vicker Hardness (MPa). A hardness test can also be used as a way to gauge the relative difference in properties of two materials. A lower hardness implies a higher ductility but lower yield strength; a higher hardness implies more brittleness but higher yield strength [1]. For the specific case of carbon steels, in general higher carbon content indicates a higher hardness. This property is explained by visualizing iron and carbon on the atomic level; more carbon atoms in the solution of iron atoms prevent the dislocation of the crystal structure.
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4.0

EXPERIMENTAL METHODS
Prior to conducting the experiment, a laboratory technician heated a furnace to ~850C and

4.1 Heat Treatment Experimental Setup placed a two gallon bucket of room temperature water (~25C) nearby for quenching purposes. 4.2 Heat Treatment Procedure The following steps were followed during the heat treatment process (see photos in Appendix C): 1. We prepared a small bullet-shaped sample of AISI 1045 carbon steel. ! 4

2. The sample was heated to 850C in the environmental furnace using a nitrogen purge holding the sample at 850C for a minimum of one hour. 3. Immediately after the sample was removed from the oven, the sample was quenched in the bucket of room temperature water until cooled. 4.3 Rockwell Hardness Testing Experimental Setup For the Rockwell hardness testing experiment, four MSC Rockwell hardness B and C calibration blocks with certified hardnesses of 42.8 B, 98.0 B, 26.7 C, 62.4 C, respectively, were used to calibrate a Wilson Rockwell Hardness testing machine (See Appendix D). Once calibrated, four small, bullet-shaped steel samples of 1018, 1018 heat treated, 1045, and 1045 heat treated steel, were tested on the machines. Because the Rockwell hardness test is considered to be coldworked, the depth of material affected during testing is on the order of ten times the indentation depth; therefore, the aforementioned steel samples were checked to confirm they were of allowable thickness. 4.4 Rockwell Testing Procedure The following steps were taken in conducting the Rockwell testing of the four calibration blocks and four steel samples (see photos in Appendix D): 1. After selecting the proper indenter for the B or C hardness test, we secured the indenter to the Rockwell Testing machine preventing any undesired movement. 2. Due to hardness differences in calibration material, Rockwell B testing requires two weights totaling 100kg to provide correct mechanical leverage while Rockwell C requires three weights totaling 150kg. Prior to testing, weights were checked to ensure correct testing adding or removing the top 50kg weight if necessary. 3. The calibration block or test steel sample was placed on the anvil, with specimen surface approximately normal to the indenter apex and the specimen firmly fixed so that it did not move or slip during indentation. The support was rigid enough to prevent permanent deformation during indentation. 4. The capstan wheel was turned until the indenter came in contact with the material. For accuracy the distance from the center of the indentation to the edge of the specimen must be at least 2.5 times the indention diameter. The distance from center to center of indentations should be apart by a minimum of three indentation diameters. 5. We continued to turn the wheel until both dials on the indicator were pointing completely up, indicating the minor load was being applied. A tolerance of 1 tick mark was an acceptable threshold for the larger dial.

6. After rotating the handle to trigger the major load, we waited until the handle came to a complete stop to ensure the load was fully applied. 7. The major load was removed by resetting the handle and we recorded the indicated hardness an Excel spreadsheet, making sure to read from the correct hardness scale. 8. The minor load was removed using the hand wheel, turning counter clockwise until the indenter tip was no longer touching the sample. 9. The sample was then removed and process repeated.

5.0

RESULTS
Please refer to Appendix E for the Rockwell Testing Results charts. We first performed

three hardness tests on each of the provided test blocks (2 each for B and C scale) and then averaged these results and compared them to the rated hardness values. With two data points for each scale we were able to plot a best-fit-line and arrive at the following equations (see Appendix F), where HRBa and HRCa refer to the actual Rockwell Hardness values (what we desire) and HRBe and HRCe are the experimental values that we measured in lab. Rockwell Hardness B Scale: !!"# ! !!!!"#$!!!"#$! ! !!!""# Rockwell Hardness C Scale: !"#$ ! !!!!!""!!!!"#$! ! !!!"!# Raw data for all of our tests can be found in Appendix G. We also present the standard deviations of each set of tests we performed. It is worth noting that the deviations of the heat-treated samples were considerably higher. We also include the estimated values for the Ultimate Tensile Strength, Brinell Hardness (HB) and Vicker Hardness (HV) which were found from tabulated values [3]. We finally estimated the Yield Strength of each sample by taking one third of the Vicker Hardness. The most significant observation to make about this data is that although the 1045 was stronger than the 1018 to begin with, the heat treated samples of both were substantially stronger than either of their non-heat treated counterparts. For both steel alloys, the heat-treating process resulted in an approximate doubling of the materials strength.

6.0

DISCUSSION
The 1018 and 1045 steel samples that we tested contain 0.18% and 0.45% carbon by weight,

respectively, and since both of these are less than 0.76% carbon, they are classified as hypoeutectoid. Both non-heat treated test samples should have had similar microstructures because they were both hypoeutectoids with carbon contents above 0.022%-wt (where the carbon component becomes trivial.) According to the phase diagram of carbon steel (See Appendix A), which assumes slow cooling, a hypoeutectoid will be a mixture of !-ferrite and cementite phases. However due to uncertainty of the how the testing samples were created, the following three ! 6

microstructures may be present in the untreated steel: (1) Martensite, if rapidly cooled; (2) Bainite and/or Ferrite if cooled slowly; or (3) Bainite, Ferrite, or Pearlite, if cooled very slowly. In this experiment, the 1018 and 1045 steel samples were raised to a temperature of 850C, well above the critical temperature of 748C, meaning they consisted entirely of the austenitic or "phase. They were then quenched to approximately room temperature (~25C) in just a few seconds. Because of this rapid cooling, the material did not have enough time to go through equilibrium phase transformation. Instead, the austenite phase turned completely into Martensite, skipping the pearlite knee present in the TTT diagram (See Appendix B). The most important result to take away from this lab is that the heat treated (HT) samples were harder than the non-heat treated (NHT) samples for both the 1018 and 1045 steel samples. The heat treatment resulted in a 94% and 127% increase in yield strength for the 1045 and 1018 steel samples respectively. Therefore, our hypothesis has been confirmed that heat treatment resulting in a Martensitic phase transformation will increase the hardness of a steel sample. Due to its tightly packed crystal lattice, Martensitic steel is the strongest form that steel can take [4]. Because of how rapidly our samples were cooled (just a few seconds), there was no time for other phases of steel, such as Bainite, Ferrite or Pearlite to form. The Carbon atoms did not have any time to diffuse as they were trapped in the tightly contracting crystalline structure, resulting in a much harder, but also more brittle material. Looking at a TTT diagram (see Appendix B), it is clear that when steel is rapidly cooled (approximately 1 second), it avoids the pearlite knee which would signify the formation of other phases. We also saw that the 1045 sample was stronger than the 1018 sample, both before and after heat treatment. This is due to the higher Carbon content, since the Carbon atoms in the crystalline lattice interrupt and help prevent the atomic dislocations that occur when steel is loaded and undergoes plastic deformation. However, because the material is less ductile, and more resistant to small plastic deformations, it is more likely for the crystal lattice to break apart and for the material to shatter under loading. This is the trade-off of the increased strength. Because Martensite is the hardest phase that our steel samples can take, it would not really be possible to have achieved a harder sample by altering our heat treatment process and we would not really be able to strain harden it because the high brittleness makes it likely to break. Perhaps if we had tempered the samples to make them more ductile, we would have been able to strain harden them, and this might have resulted in a harder sample. There are a number of ways that error could have entered our results. We were using manual Rockwell Hardness Testing Machines, so there was the possibility of each trial being slightly different in its execution. However, we were careful to keep each new indentation far ! 7

enough away from both the edge and from the other indentations so as to avoid possible affecting our readings. If the plastic region around our new indentation overlaps that of a previous indentation, the strain hardening that resulted from the previous test could cause the new reading to be too high [4]. As a rule of thumb, we used three times the width of an indentation as the minimum distance between indentation tests [1]. Perhaps our most significant possible source of error was in taking readings from the dial. We rounded each of our results to the nearest half value, so our measurements could be off by as much as 0.5. Despite this, the conclusions that we draw from our test results are still valid, because the margin of error in our results is much smaller than the approximate doubling in hardness that we observed.

7.0

CONCLUSIONS
By completing this lab we learned that both carbon percentage and heat-treatment

significantly affect the material properties of steel. Rockwell hardness tests with AISI 1018 and 1045 steel samples indicated that the higher carbon content helped the steel resist plastic deformation, making it harder or more difficult to indent. In addition, comparing heat-treated samples with their non heat-treated counterparts showed that the heat-treatment process results in significantly higher strength and hardness. We concluded that this higher strength was due to the steels phase transformation to a martensitic structure during the heating and quenching process. 7.1 Lessons Learned In future labs we should be more thorough with documenting the experiment and asking questions to the lab technician. Because this was the first lab, we had to familiarize ourselves with the procedures and were less concerned with the report writing aspect of the lab. Additional information and pictures from the experiment may provide for a more detailed and comprehensive lab report. Furthermore, having more experience with using the equipment may reduce human error and increase overall accuracy of results and data reading.

8.0

REFERENCES

[1] Kyriakos Komvopoulos, Mechanical Testing of Engineering Materials. (USA: Cognella, 2011). [2] James F. Shackleford, Introduction to Materials Science for Engineers, 7th Edition (Upper Saddle River, NJ: Pearson Prentice Hall, 2009). [3] Hardness Conversion Chart, Retrieved from http://www.carbidedepot.com/formulashardness.htm [4] William F. Hosford, Mechanical Behavior of Materials. (New York, NY: Cambridge University Press, 2005).

9.0 9.1

APPENDIX Appendix A Fe-C Phase Diagram

9.2

Appendix B TTT Diagram of Eutectoid Carbon Steel

10

9.3

Appendix C Heat Treatment Photos

The steel sample being pulled out of an environmental furnace

The steel sample being quenched in water

11

A before/after shot showing the heat treated sample (black) and the untreated sample (silver)

12

9.4

Appendix D Rockwell Hardness Testing Photos

Rockwell hardness testing C calibration blocks Rockwell hardness testing C calibration blocks

A Wilson Rockwell Hardness Testing Machine

13

The different parts of a Rockwell test machine: 1: Crank Handle 2: Indenter tip "#!$%&'(!)(*+,! -#!.*)/+*%!01,,(! 2#!34*((!)5'%+,6! 7#!8*69,!)5'%+,6!

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9.5

Appendix E Results of Rockwell Testing Experiment

Scaled Sample Scale Rockwell Hardness Value 1018 Steel NHT B C B C B C B C 82.2 0.0 91.4 8.9 107.8 36.2 113.5 37.7 0.4 0.0 0.2 0.7 0.7 2.3 1.5 1.4 Standard Deviation

Tensile Strength (MPa) 517

HB (kg/mm2) 153

HB (MPa) 1500

HV (kg/mm2) 160

HV (MPa)

Yield Strength (Mpa) 523

1569

1045 Steel NHT 1018 Steel HT

628 1110

185 344

1814 3373

192 363

1883 3560

628 1187

1045 Steel HT

1180

353

3462

372

3648

1216

15

9.6

Appendix F Actual Values of Calibration Blocks vs. Experimental Results

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9.7

Appendix G Laboratory Test Results

Deviation from Standard Calibration Test Scaled Deviation Standard Indenter Load Result 0.4 3.7 1/16" ball 100kg 0.2 0.8 1/16" ball 100kg 0.4 0.4 0.2 1.5 0.7 1.4 0.4 0.7 0.0 2.3 read <0 -0.2 -0.4 diamond 150kg diamond 150kg 1/16"ball 100kg 1/16" ball 100kg diamond 150kg diamond 150kg 1/16"ball 100kg 1/16" ball 100kg diamond 150kg diamond 150kg 91.4 113.5 8.9 37.7 82.2 107.8 0.0 36.2

Sample Test 1 Test 2 Test 3 Calibration Test Block 42.8 B scale 46.0 47.0 46.5 Calibration Test Block 98.0 B scale 98.5 99.0 99.0 Calibration Test Block 26.7 C scale Calibration Test Block 62.4 C scale Steel 1045 NHT B scale Steel 1045 HT B scale Steel 1045 NHT C scale Steel 1045 HT C scale Steel 1018 NHT B scale Steel 1018 HT B scale Steel 1018 NHT C scale Steel 1018 HT C scale 26.5 61.5 27.0 62.0 26.0 62.5

Average of three tests 46.50 98.83 26.50 62.00 90.17 113.50 9.00 38.00 80.50 107.50 0.00 36.50

90.0 90.0 90.5 112.0 113.0 115.5 8.5 39.0 10.0 39.0 8.5 36.0

81.0 80.0 80.5 108.0 108.0 106.5 0.0 39.0 0.0 33.5 0.0 37.0

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