Laboratory Report

Metallography and Heat Treatment

Abstract
As not all the native properties of pure metals are useful in certain contexts, it is important that engineers understand how they can be modified. Heat treatments affect the structure of metals and hence their properties by hindering or assisting in creating imperfections in their crystalline structures. As a result, it is important to understand the theory and results obtained from heat treatment processes as they can be costly if used inappropriately. Alloying two or more metals together can result in an improvement of the mechanical properties of the final alloy. This is due to the different properties (e.g. strength, ductility, hardness) of the base metal and its alloying addition. Similarly, cold working can result in an increase in mechanical properties like strength and hardness due to an increased density of imperfections in the metal. This report considers the effects of factors like heat treatment, cold working and alloying additions by observing quantitatively their effects on a metals hardness and qualitatively on its crystal structure.

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Introduction
The purpose of this report is to demonstrate the uses of modifying elemental metals to obtain useful engineering materials. Specifically, it will explore the effects of heat treatments, alloying and cold working on the mechanical property of hardness for several different forms of metal. From these hardness measurements, the tensile strength of each specimen may also be estimated. The report will also demonstrate the theory behind the changes in mechanical properties brought about by these treatments. This will be illustrated using a microscopic study of several different metallic specimens which have undergone different treatments to modify their mechanical properties.

Background
Hardness is defined as the ability of a material to resist deformation in the form of surface indentation or abrasion (Callister and Rethwisch, 2010, 174). Similarly, strength is the ability of a material to withstand a load without fracturing. Strength and hardness in metals are related in the sense that they both are largely determined by the crystal structure of a metal. The crystal structure of a metal is seldom perfect; line defects occur where a plane of metal atoms may be incorrectly aligned and hence a dislocation is formed. According to Callister and Rethwisch (2010, 199), deformation in metals corresponds to the motion of a large number of dislocations, giving rise to a change in the shape of the solid as its crystal structure is rearranged. Hence, the properties of hardness and strength are related to the ease with which dislocations can move through a metals crystal structure. The difference between a wrought and cast alloy is the way in which it was formed. As explained by SECAT Inc. (Aluminium Technology 2012), wrought alloys have been subjected to cold working (e.g. hammering into shape) while cast alloys were formed by solidification into a mold. As described by Callister and Rethwisch (2010, 216), cold working results in the formation of more dislocations in a crystal structure. These dislocations have a repulsive force on each other and hence begin to hinder their movement (increasing hardness and strength) throughout the crystal structure. Thus, as cold working is applied to a metal, its hardness and strength increase. As metals cool down, grains of perfect crystal structure grow against each other (see Figure 2). If a cast metal is allowed to cool at equilibrium conditions (i.e. slowly), the grains grow from the cooler outside towards a centre point (Figure 2, panel a). If the metal is rapidly cooled, both the outside and core are cooled quickly forcing the inner and outer grains to grow simultaneously. This creates the disordered structure show in Figure 2, panel b. If a steel is rapidly cooled (quenched), it produces a structure of iron known as martensite which is extremely brittle and hard. The hardenability of a steel is the rate of cooling (quenching) required to produce a completely martensitic (hard) structure (Hardenability 2004). Thus a steel is considered hardenable if it requires a relatively low cooling rate to induce martensite and thus hardness. The Jominy Bar test measures the hardenability of a metal by quenching a bar from a certain face. The distance away from that face then is proportional to the rate of cooling occurring at that position (e.g. further away from the quenched face relates to a slower cooling rate). 2

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An important relationship between hardness, strength and the crystal structure of a metal is explained by the Hall Petch equation (Callister and Rethwisch, 2010, 213): y = 0 + kyd-1/2 where y is the yield strength, 0 and ky are constants dependent on the material being tested and d represents the average grain diameter. As d (grain size) decreases, the yield strength y, (value at which plastic deformation commences) increases. As grains are oriented in different directions, dislocations passing through grain boundaries are forced to change direction, hindering their movement. This increases the strength and therefore the hardness as shown in the equation. A slip plane is described as the plane over which a dislocation would preferably move (Callister and Rethwisch, 2010, 202). The presence of an alloying addition in solid solution with a base metal can result in the disruption of these slip planes and hence the inhibition of dislocation movement.
Dislocation motion Slip Plane Dislocation motion Slip Plane

(a)

(b)
Figure 1: Dislocation movement in (a) pure metal (b) solid solution

Figure 1 panel (a) depicts the motion of dislocations along a slip plan in a pure metal. As the atoms are all the same size, dislocations can slide along the plane relatively freely. Panel (b) shows the orientation of the dislocation movement in a substitutional solid solution. As the alloying addition (blue atom) is of different size to the other native red atoms. The dislocation must move in a curved path, hindering its motion. Thus solid solutions give rise to strength and hardness (less dislocation movement). Another method of hardening a metal is known as age or precipitation hardening. First a metal is heated to liquid phase. It is then quenched to retain the soft, ductile structure (coarse grains) obtained at high temperatures. While the ductility of the material is desirable, the lack of strength and hardness is not. Over time, through the process of metallic diffusion, the structure will eventually precipitate the normal weaker, ductile room temperature phase cooled at equilibrium conditions. This will occur at the grain boundaries of the quenched phase creating ultra-fine grains (quenched and precipitated). This leads to harder dislocation movement and higher strength and hardness according to the Hall Petch equation. At this point, the metal is in its optimum condition, being hard, strong and relatively ductile. As time progresses, the metal may become overaged where the precipitates dominate the structure and the grain size increases. This causes a related fall in the strength and hardness. This process can be accelerated by heating the metal slightly ~100-200C after it has been quenched, accelerating the metallic diffusion process to the optimum condition (high strength, hardness and ductility).

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Experimental Procedure
Part A - Metallography 1. A sample wrought copper in a microscope slide was inserted into the microscope for study 2. A clear image of the copper samples grain structure was obtained and copied into the lab notes 3. The magnification at which this image was obtained was also noted 4. This process of illustration using microscopic observation was repeated for two additional samples; slow cooled cast aluminium and rapid cooled cast aluminium 5. An observation of the crystal structure of wrought 60/40 brass was obtained through a display on a provided television (magnification was provided as x100) Part B Age Hardening and Solid Solution Strengthening 1. The Rockwell A hardness of several specimens of Aluminium Alloy 2011 which had underwent solid solution strengthening with 4.0% copper at 525C followed by age hardening of a specified time (0 to 240 minutes) at 180C were tested (see hardness testing procedure below) 2. Three trials were taken from each and a reliable average obtained 3. The hardness was plotted as a function of ageing time Part C Effect of Rate of Cooling 1. A Jominy Bar of Plain Carbon Steel (AISI 1040) and Alloy Steel (AISI 4340) was prepared and heated to ~900C in a furnace 2. These were then placed in a water fixture so that their bases were quenched by a fountain of water 3. The Rockwell C hardness at increasing increments from the quenched end of each Jominy Bar were taken (see hardness test procedure below) 4. These values plotted against the distance from the quenched end yielded a hardenability curve Hardness Testing procedure 1. The sample was placed on the Rockwell Hardness tester between the diamond testing tip and the anvil 2. The compression lever was wound until the two hardness pointers were vertically upwards (taking care not to exceed this level) 3. The testing lever was pressed and the final Hardness value was recorded 4. The sample was released from the hardness tester

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Results
Part A - Metallography
Centre point

Slow Cooled Cast Aluminium

Rapid Cooled Cast Aluminium

x1

(a)

x1

(b)

Wrought Copper

Wrought 60/40 Brass

x150

(c)

x100

(d)

Figure 2: Microscopic View of Grains in metals of various treatments

Figure 2 shows the results of the microscopic study into the grain size of four metal samples. In slow cooled cast aluminium; panel (a), under a magnification of x1, the grains appear to be radiating outwards from a centre point labeled with the red dot. This is indicative of the grains growing from the outer edge of the metal to the centre point. Panel (b) represents cast aluminium that has been rapidly cooled. Here, the grains exhibit no definite structure and appear to be randomly oriented. This indicates that the grains were all growing at the same time; the temperature differential between the outer surface and core was minimal. Panel (c) illustrates the grains in wrought copper which are relatively fine (indicated by the high magnification of x150) compared to the cast samples (x1). It is single phase; each grain is composed of the same FCC copper structure. Panel (d) shows the multiphase structure of 60/40 brass. The grains are similarly finer than the cast samples, however, are composed of two phases. The dark areas represent grains of solid solution (limited Cu dissolved in a BCC Zn crystal structure) while the lighter areas are grains of solid solution (limited Zn dissolved in a FCC Cu crystal structure).

Engineering Materials 100 Part B Age Hardening and Solid Solution Strengthening

Hardness vs Ageing Time

39 37 35 33 31 29 27 25 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 Ageing Time (mins)
Figure 3: Plot of Rockwell Hardness A vs Ageing time of Aluminium Alloy 2011

Figure 3 depicts the average Rockwell A hardness as a function of ageing time of the aluminium alloy samples. The red line represents the trend that occurs as the ageing time increases. From no ageing (0mins) to approximately 30mins, the hardness uniformly rises up to a maximum value of 39 HRa. Following this limit, the hardness decreases and becomes a constant value of 34HRa from 52mins onward. Part C Effect of Rate of Cooling
70 60 50 Hardness (HRc) 40 30 20 10 0 0 5 10 15 20 25 30 35 40 45 Distance from Quenched Face (mm) 50 55 60 AISI 1040 AISI 4340

Hardness (HRa)

Figure 4: Plot of Rockwell Hardness C vs Distance from Quenched Face (base of Jominy Bar)

Figure 4 shows two trends, the hardness of AISI 4340 (Alloy Steel) remains at an almost constant (within the bounds of experimental error) 57HRc all along the Jominy Bar. In contrast, the hardness of the AISI 1040 (Plain Carbon Steel) decreases the further away the hardness is tested from the quenched face. It falls steeply from 54HRc to 29HRc within the first 10mm away from the quenched face of the Jominy Bar. Following this, the hardness stabilises, decreasing at a slower rate (flatter gradient) as the hardness is tested further along the Jominy Bar. 6

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Discussion
Part A Metallography Panel (a) of Figure 2 clearly shows the process of grain growth from the cooler outside inwards towards the hotter centre point. This is consistent with the theory as the outside skin of a heated metal will cool faster than the inner core when cooled slowly at equilibrium conditions. Similarly, panel (b) shows how grains grow at the same time and are thus arranged with no apparent order when a metal is quenched rapidly to room temperature. Panel (c) and (d) depict how wrought materials have much finer grains (higher magnification) due to cold working. This supports the theory and explains why cold worked materials exhibit higher strength and hardness but are brittle. Part B Age Hardening and Solid Solution Strengthening Figure 3 shows that up to a limit of approximately 30mins ageing time, the hardness of the Aluminium Alloy was increased. This supports the theory espoused by Zerger (2007) that as a quenched metal ages, ultra-fine grains of its normal equilibrium phase are precipitated at the grain boundaries, increasing its strength and hardness. Following this limit, overageing occurs (quenched phase decreases in concentration relative to equilibrium phase) and the hardness values fall. Part C Effect of Rate of Cooling As both samples represented in Figure 4 underwent the same heat treatment, it is appropriate to directly compare their hardenability. At the rate of cooling provided by the Jominy Bar test, the AISI 4340 (Alloy steel) has had its entire length hardened to the martensitic phase. In comparison, the AISI 1040 (Plain Carbon steel) has a decreasing hardness the further distance measured from the quenched face. As the distance from the quenched face is directly proportional to the cooling rate, it can be observed that the carbon steel (AISI 1040) required a higher cooling rate to obtain a martensitic (hard) structure than the Alloy steel (AISI 4340). This indicates that the Alloy steel (AISI 4340) is more hardenable than the carbon steel (AISI 1040) as it requires a lower cooling rate to obtain the hard martensitic phase.

Conclusion
This experiment has demonstrated the beneficial effects that various treatments can have on the mechanical properties of metals. Most prominently, the effect of heat treatments, cold working and alloying have been observed on the property of hardness. This means that the properties of metals can be modified through these treatments to obtain more useful engineering materials suitable to certain contexts (e.g. airplanes, oil rigs). The dislocation and crystal structure theory behind the bolstering of hardness has also been explored, demonstrating on a microscopic level how materials can be modified to produce macroscopic properties which can then be used by engineers to solve problems.

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References
Callister, William D. and David G. Rethwisch. 2010. Materials Science and Engineering: An Introduction. Hoboken: John Wiley & Sons, Inc. Aluminum Technology, Aluminum Testing, Aluminum Research. 2012. SECAT Inc. http://www.secat.net/answers_faq.php. Hardenability. 2004. MATTER Materials Science and Engineering Education. http://www.matter.org.uk/steelmatter/metallurgy/7_1.html. Serder Z. Elgun. 2007. Age Hardening. Farmingdale State University. Accessed May 14, http://info.lu.farmingdale.edu/depts/met/met205/agehardening.html.

Appendix Lab Notes