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NANYANG TECHNOLOGICAL UNIVERSITY School of Materials Science & Engineering MS2082 Second Year Undergraduate Experiment

Laboratory Manual For EB3 Precipitation Hardening in an Aluminium Alloy

Laboratory: MSE Undergraduate Lab Location: N4-B4-W101, Rm 4

Lab manual prepared by A/Prof. Raju V. Ramanujan, 2012 1. Objectives To understand the principle of precipitation hardening. To acquire the basic skills to operate a hardness tester and to obtain hardness values using the tester. To understand the effect of aging heat treatment on mechanical properties of materials. To reinforce the understanding of the relationship between structure and mechanical properties through hands-on experience.

2. Introduction In 1911, Wilm discovered that Al-Cu alloys harden during aging after quenching. This was the starting point of a new technique for improving the mechanical properties of metals. Especially for Al, thanks to this technique, its alloys have become the preferred alloys for applications in the field of aerospace transport. Today, precipitation hardening has become a common practice in metallurgy. It does not apply only to Al-based alloys. Table 1 below provides examples of precipitation hardened alloys. In this experiment, we propose to highlight the hardening by precipitation of a second phase in an Al-4% Cu alloy. Table 1 Precipitation hardenable alloys. Metal base alloy Composition (weight %) Precipitates


Copper Nickel Iron

2024 6061 7075 Cu-Be Nimonic 105 Maraging steel

Al-4.5 Cu-1.5 Mg-0.6 Mn Al-1.0 Mg-0.6 Si-0.25 Cu-0.2 Cr Al-5.6 Zn-2.5 Mg-1.6 Cu-0.2 Mn-0.3 Cr Cu-2.0 Be-0.5 Co Ni-20 Co-15 Cr-5 Mo-4.5 Al-1 Ti-0.15 C Fe-20 Ni-9 Co-5 Mo-0.7 Ti-0.1 Al

S' Al2CuMg ' Mg2Si ' MgZn2 zones ' Ni3TiAl FeMo

3. The treatment of precipitation hardening is done in three steps 3.1 Solutionizing: The alloy is heated to a temperature as high as possible (for Al about 500 C), to allow the dissolution of the elements that cause the hardening (Fig. 1). To avoid the risk of partial

melting, the temperature must remain below the eutectic temperature and melting temperature of the intermetallic phases present. Indeed, partial melting of a component of the alloy makes the piece unusable. The duration of maintaining the temperature is about 30 min. As the final properties depend very strongly on the temperature and the duration of solution heat treatment, one must check with the manufacturer for optimum results. For some alloys of the Al-Cu series, it is recommended to control the temperature with an accuracy of 5 C.

Fig. 1 Equilibrium phase diagram of Al-Cu alloys showing the solubility limit and region of precipitation of GP zones and ", ' and phases (= Al2Cu).

3.2 Quenching: Quenching is done to maintain the components in metastable solution. The rate of cooling required depends very strongly on the alloy. The Al-4% Cu alloy must be cooled to 200 C in less than 5 to 15 s. Below 200 C, the cooling rate is more critical. In Al-Zn alloys containing no Cu, the phase separation is slower and can be cooled in 5 to 20 min. It follows that the AlCu alloys require water quenching, while Al-Zn alloys can be cooled in air. The mechanical strength of alloys in this state is due only to solid solution hardening and is only mediocre. Very slow cooling allows the phase separation of the solution. The precipitates become relatively large and contribute little to hardening. The mechanical properties are close to that of Al. 3.3. Aging: These operations aim to realize phase separation of the supersaturated solution. Apart from the phases that precipitate (compositions and crystallographic details), the reaction proceeds similarly in different alloys. We take here the Al-Cu alloy with 4% Cu as an example.

Above 500 C, the solid solution of Al + 4% Cu is in equilibrium (Fig. 1). Below this temperature, the intermetallic compound is formed of Al2Cu by the mechanism of nucleation and growth. The new grains that appear have a crystalline structure different from that of the matrix, and there is no relationship between the crystallographic axes of the two networks. The formation of such a grain requires high thermal activation energy to compensate for the high interfacial energy at the nucleation stage. The interfacial energy is particularly high for an interface between two different crystal lattices. The atoms forming the interface between the two crystals cannot be arranged so they are all separated by their normal distance. The binding energy between these atoms is reduced and decreases the cohesive energy of the alloy. The decrease in this energy, calculated per unit area of interface, is precisely the interfacial energy. At room temperature the thermal fluctuations have amplitudes too small for nucleation, a new grain can arise only at elevated temperatures. Of all the possible types of interfaces, the one whose interfacial energy is the lowest is that for which the new composition has coherent/similar crystallographic orientation with the matrix. We can describe this as a crystal with a local variation in composition or as two crystals between which there is a crystallographic coherence. They are called Guinier-Preston zones. Diffusion at low temperature is extremely slow; the GP zones are necessarily very small. In fact, they are so small that they can only be observed by high resolution imaging techniques e. g., Transmission electron microscopy (TEM) and High resolution transmission electron microscopy HRTEM. In Al-Cu alloy, they consist of one atomic layer of about 30 by 30 Cu atoms arranged along the crystallographic planes of (002) (Fig. 2a, bright field TEM and Fig. 2b, HRTEM image). At higher temperatures, other forms of precipitates appear. At 150 C, the precipitates become larger. There is a change of crystal structure, while still remaining in crystallographic coherence. These GP II zones, as they are now called, consist of the metastable " Al2Cu phase. Between 200 and 300 C, platelets are formed of the ' phase which has the crystal structure of Al2Cu but still maintains its crystallographic orientation with the Al matrix. Above 300 C, nucleation and growth produces m size grains. These grains are made up of the phase, which is the equilibrium phase of Al2Cu (tetragonal). Table 2 summarizes the sequence of precipitation. Solid solution ( phase), is always present, Cu is depleted gradually from the matrix when approaching the equilibrium microstructure + . Table 2. Sequence of precipitation and the effect of precipitation in the Al-4%Cu alloy. Crystallography tetragonal incoherent a (nm) 0.607 c (nm) 0.487 Remark Overaging, reduces corrosion resistance Overaging

' "=G.P. II

tetragonal partially coherent tetragonal coherent coherent






G.P. I



Fig. 2 G.P. zones observed by (a) bright field TEM and (b) High-Resolution TEM. Note that the GP zones are only a few Angstrom thick. Hardening of the alloys is optimal when both GP I and GP II zones occur, i.e. coherent and ultrathin precipitates. Coalescence, which occurs above 200 C, decreases the yield strength and tensile strength, this phenomenon is called over-aging. To arrive at the optimal mechanical properties, aging takes 5 to 8 days in the Al-Cu and Al-Mg2Si alloys (Fig. 3). Heating between 150 and 200 C can achieve optimal aging in 4 to 24 hours (depending on the alloy).

Fig. 3 Aging AlCuMg1 (4% Cu 1% Mg) alloy at different temperatures after water quenching.

Fig. 4 Aging AlZn4.5Mg1 alloy after water quenching and cooling in the air. Homogenization temperature 480 C. Note the time scale. 4. Hardening Mechanisms Solid solution hardening that occurs immediately after quenching increases with concentration of elements in solution. Nevertheless, with 4% Cu in Al, this effect is small (Table 3), and disappears with the precipitation of Cu rich precipitates. Precipitation hardening When the particles are harder than the matrix, dislocations cannot penetrate the precipitates. They are forced to circumvent them (Orowan mechanism Fig.5). The critical shear stress in the slip plane of dislocation c is calculated, in the same manner as that of a Frank Read source.

c =

Gb d

Here G is the shear modulus, b the Burgers vector and d the average distance between particles. We deduce that the strength is greater when the distance between the particles is small. However, below a critical size, they can no longer resist a shear stress c and yield before the dislocation looping. The new critical shear stress p, depends on the cross sectional area of the particles and the mechanical properties of the matrix and particles.

Fig. 5 Interaction of dislocations with hard particles (bypass).

Fig. 6 Interaction of dislocations with coherent precipitates.

Shearing of the precipitates GP zones which form at the beginning of the precipitation are very small and they are coherent with the matrix (Fig. 6). Their resistance to deformation increases with their size. The strength increases with the progression of transformation to tetragonal particles (") and semicoherent particles ('). TEM micrographs of representative " and ' precipitates are shown in Fig. 7. Hardening increases until the bypass mechanism becomes competitive and c = p. In this state it is optimally aged. Increasing aging time causes coalescence of GP zones and ' and the appearance of other phases with coarser grains. The increase in the separation of the particle d facilitates the circumvention and softens the metal (overaging). The curves show the tensile strength, yield strength and hardness as a function of time (Figs. 4 and 8).

Fig. 7 Bright field TEM micrographs of theta' (a) and theta" (b) precipitates in Al-Cu alloy. Note the difference in the size of the precipitates with Fig. 2.

Fig. 8 Hardness as a function of aging time at 130 and 190 C for Al-Cu binary alloys.

Hardening To further increase the yield and tensile strength, they can be cold worked. The combined effect of work hardening and precipitation hardening is represented in Fig. 9. In practice, it should be limited to a few percent of cold working.

Fig. 9 Hardening of the Al-4% Cu by the combined effect of work hardening and precipitation hardening.

5. Experiment Determine the aging curve (hardness v/s time) for the Al-4% Cu alloy. Hardness measurements performed using a Vickers hardness machine. Procedure Homogenize the samples in the homogenization furnace which is preheated to 500 C. After 5 hours, quench the test samples in a tray of water. It is important to reduce the transit time between the oven and tray to the minimum necessary for the transfer. Put these specimens in a preheated oven at 250 C. Take out the specimens from the oven after 10, 20, 40, 80, 180, and 480 min.

Measure the hardness HV of the specimen in peak aged commercial materials (received from supplier), quenched and aged conditions, at least 3 measurements per sample.

6. LAB REPORT Students are required to submit a Formal Report or a Short Report / Log Sheet. The Formal Report will usually contain a statement of the experiment objectives, the theory, the equipment used, experimental procedure, experimental observations, results and discussion, conclusions, and references you have read. Use your own language and be concise. The report is not expected to be excessively long since an overly long report may reflect an inability of the student to condense his thoughts and to decide between relevant and trivial information. Difficulties encountered while performing the experiment, sources of error, comparison with results predicted by theory, answers to questions posed in the instruction manual are to be included in the report. Submit your Formal Report within two weeks after the experiment. A Short Report / Log Sheet reports only on essential information on experimental procedure and results, and answers to questions posed. Submit your Short Report / Log Sheets within one week. Plot the aging curves for the Al-4% Cu alloy, write a lab report based on the results obtained and discuss the results based on the provided background. 6. LEARNING OUTCOMES After completing the experiment, you should be able to understand how precipitation hardening occurs. design heat treatment procedure for precipitation hardening of alloys. understand the effect of aging heat treatment on mechanical properties of materials and the general relationship between structure and mechanical properties. operate a hardness tester skillfully and to obtain valid hardness values using the tester.

7. REFERENCES R.E. Smallman and R. Bishop, Physical Metallurgy and Advanced Materials, 7th Edition, Butterworth-Heinemann, 2007. (TN690.S635 2007, E-Book) Lab manual, Ecole Polytechnique Federale de Lausanne (EPFL) (Switzerland). Materials Sci. and Engg., W.D. Callister, 6th edn. Structure of Metals, C. Barrett and Massalski. Structure and Properties of Engineering Materials, D. Henkel and A.W. Pense, 5th edn. (2001). Intro. to Engg. Materials, B.K. Agrawal, Tata McGraw Hill, 1988.