DEPARTMENT OF MECHANICAL ENGINEERING ALL Sections must be completed using Block Capitals or typed

CODE AND TITLE OF COURSEWORK Course code: MECH 1006 Title: METALLOGRAPHY & MICROSTRUCTURE 1 LAB N

STUDENT NAME: LIU CHUN KIT, JOHN

DEGREE AND YEAR: MENG IN MECHANICAL ENGINEERING YEAR 1 (11/12 INTAKE)

LAB GROUP: 10

DATE OF LAB. SESSION: 6 MAR 2012

DATE COURSEWORK DUE FOR SUBMISSION: 27 APR 2012

ACTUAL DATE OF SUBMISSION: 25 APR 2012

LECTURERS NAME: DR ADAM WOJCIK

PERSONAL TUTORS NAME: EUR ING FELLOWS RECEIVED DATE AND INITIALS:

I confirm that this is all my own work (if submitted electronically, submission will be taken as confirmation that this is your own work, and will also act as student signature)

Signed:
University College London, Torrington Place LONDON WC1E 7JE

Table of Contents
1. Title 2. Abstract 3. Method 3.1 Theory 3.2 Experimental Procedure 4. Results & Discussion 4.1 Specimen X18 4.2 Specimen X19 4.3 Specimen X20 4.4 Specimen X34 4.5 Specimen X31 4.6 Specimen X32 4.7 Specimen X33 4.8 Specimen X 5. Conclusion 6. References 1 1 1,2,3 3,4 5 6 7 8 9 10 11 12 13 13

1. Title This lab session encompasses the observation of prepared metallographic specimens through optical microscopes, followed by a study (for e.g. material composition, manufacturing route) of these observations through analysing the specimens microstructure. 2. Abstract The aims of the experiment are to: Understand how metallography is carried out through specimen preparation and observation of specimen structures through optical microscopes Study how the macrostructure and microstructure of these specimens affect the specimens properties (for e.g. mechanically, physically) Study how the macrostructure and microstructure of these specimens relate to the specimens composition as well as its route of manufacture (i.e. cooling rate and subsequent processes undertaken) 3. Method 3.1 Theory Steels Steels are alloys made by combining iron (Fe) and another element. Carbon (C) is the most widely used alloying element and examples of other alloying elements used are manganese, chromium and tungsten. For this laboratory session, only steels of iron and carbon will be studied. With increasing percentage composition by weight of carbon in iron, the steels are categorized into low (0.05 0.15%), mild (0.16- 0.29%) and high (0.30 2.00%) carbon steels. Subsequently, steels with a carbon content above 2% are considered as cast iron due to their lower melting point and ease of forming in castings. The important and unique feature of a steel phase diagram is that it has an eutectoid reaction. This reaction is a phase transformation which involves no liquids and generates a layered arrangement of phases that are similarly observed from eutectic reactions. The various phases present in the steel eutectoid reaction are austenite, ferrite and cementite. Austenite is a solid solution of interstitial carbon atoms in face centre cubic (FCC) iron and upon cooling becomes ferrite. Ferrite is also a solid solution but instead with a low interstitial carbon content in body centre cubic (BCC) iron. Cementite is an intermetallic compound of Fe3C formed when the iron and carbon chemically react. The eutectoid reaction occurs at a temperature of 723C and at a composition of 0.8% carbon where solid single-phase austenite cools and forms a double phase solid of ferrite and cementite. At the eutectoid composition the whole microstructure is layered. By varying the composition of carbon, the amount of primary ferrite/cementite and lamellar arrangement of secondary ferrite + cementite can be altered. The layered eutectoid arrangement of ferrite and cementite is also known as pearlite. Specimens with varying carbon content giving hypoeutectoid, eutectoid and hypereutectoid steels are examined in this lab and will be discussed later. Brass Brass are alloys made by combining copper (Cu) and zinc (Zn), commercially brass

is produced with up to 45% of zinc content. Brass is a substitional alloy with zinc atoms substituiting into the copper lattice for improved mechanical properties. Brass is generally categorised into two categories of alpha brass and alpha-beta brass. Alpha brass has a single phase microstructure which is soft and ductile, and is found in brasses with less than 35% of zinc content. Alpha-beta brass has a two phase microstructure which contains both the alpha phase and hard beta phase which results in a strong and less ductile brass. The alpha-beta brass is found in brasses with a zinc content above 35%. Cold Working Cold working also known as work/strain hardening is the process of strengthening a metal by plastic deformation. The metal is strengthened due to the dislocations of the crystal structure within the material after it has experienced plastic deformation. More specifically, as the plastic deformation creates dislocations in the metal and as the dislocations increase, the material begins to create a resistance to subsequent dislocations which therefore make it harder and more able to resist deformation. In addition, cold working also exhibits the Hall-Petch effect where the grains are compressed into smaller grains sizes. These smaller grain sizes combined with the disorientations amongst the deformed grains require more force to dislocate the microstructure resulting in higher yield stress. As the material is worked in this process, the yield stress is improved however it also results in a decrease in ductility. Annealing A solution to metals that have become brittle through processes such as cold working is annealing. Annealing is essentialy a heat treatment on the material that causes change of the materials properties such as improved ductility. The process of the heat treatment (approximately at 60% of its melting point) allows diffusion of the atoms within the solid state that allows the materials to restore its microstructure to an undeformed state, which gives the material its improved ductility. More specifically, the annealing process is disected chronologically into the three stages of recovery, recrystallisation and grain growth. Recovery is the stage where internal stresses are reduced by the removal of crystal defects such as dislocations. Recrystallisation is where the strain-free grains begin to nucleate and grow to replace those grains that have been affected by internal stresses. Lastly, grain growth occurs when recrystallisation is complete, grains begin to grow and microstructure coarsens due to the reducing grain boundary areas. Apart from attaining the critical temperature for a material to start diffusion, the annealing process also comprises of controlling specific durations for holding the critical temperature as well as varied cooling rates to achieve the final desired microstructure. For example, cooling steel rapidly will result in a fine pearlite microstructure as compared to cooling steel slowly resulting in a coarse pearlite microstructure. Hot Working Hot working is a combined process of cold working and annealing whereby metals are plastically deformed above their recrystallisation temperature allowing deformed grains to simultaneuously re-grow into non-deformed shapes. This process works opposite to cold hardening as the final product in this case has higher ductility, lower hardness and lower yield strength. Although hot working runs a simultaneous process that gives time savings, the additional cost of manufacturing equipment to withstand such high temperatures eventually makes hot working a more costly option.

Twins Twins are crystalline defects that appear in the microstructure as a thin band passing across an individual grain and can be observed in specific FCC metals and alloys that have undergone the annealing process. Twins exhibit the same crystal structure as the rest of the grain and share the same crystal lattice points in a symmetrical manner. The thin band observed is a result of a change in crystal system during cooling from annealing where a portion of the grain that is unstable re-organises its crystal structure to a more stable state. Slip Line & Slip Steps Upon undergoing deformation, slip lines and slip steps can be seen in the microstructure of metals. Slip lines are due to the deformation of metals along a preferential direction, which is determined by the crystal structure. Slip steps are caused by the slippage of crystals along the preferential directions, which result in the formation of steps. Even when these features are polished away in preparation for metallographic examination, etchants can be used to reveal traces of its presence. Banding Banding can be seen on metals and can be observed from its fibrous texture appearance. Banding is caused by deformation of two-phase materials that have been cold worked (for e.g. rolled) together which apart from elongating the grains, it also bands the phases together. Various mechanisms are responsible for this banding effect and they vary depending on the metal examined. With the understanding of the several microstructure features above, it gives valuable clues as to how each specimen was manufactured and will aid in the analysis of the specimens in this lab. 3.2 Experimental Procedure The experimental procedure involves the following 5 steps: 1. Cutting the material The material is cut using abrasive blades (from diamond tip cutters to hardened steel saws) around its area of interest as well as cut to a suitable size for easy handling. Depending on the material, various abrasive blades, speed settings, loads and coolants are used to ensure that the microstructure is not altered so as to not provide false metallographic characterization. 2. Grinding The surface of the specimen is grinded by using a rotating disc covered typically with silicon carbide paper (from coarse to fine grades) and water. The water acts as a lubricant as well as a means to remove grinded particles. Every time the silicon carbide surface grade is changed, the specimen will be rotated with the orientation of the scratches from the previous grade to be perpendicular to the rotation direction. This allows the lab personnel to easier observe when coarser scratches from the previous grade have been removed. This process is repeated until the final typical grade of 1200 grains per square inch silicon carbide surface is used and that all surface blemishes have been removed, surface is flat and scratches are all in the same direction. Thereafter, the specimen is washed with water followed by alcohol and finally drying before moving to polishing.

3. Polishing The surface of the specimen is polished by using rotating disc covered with soft cloth impregnated with diamond particles and an oily lubricant. The diamond particles used start with a size of 6 microns and gradually lowered to a size of 1 micron. Upon reaching the 1 micron polishing stage, polish is continued until all grinding scratches have been removed before stopping. 4. Etching It is essential that etching is carried out on a clean grease free specimen surface so as to allow the full surface of the specimen to be attacked evenly. To achieve this, the specimen is washed with soapy water followed by alcohol (or distilled water) and finally drying in the air. Next, etching is commenced by immersing the specimen surface in an etching solution appropriate for that material for a specific duration of time depending also on the material. The function of the etchant is to first remove chemically the thin layer of highly deformed surface (caused from the grinding and polishing) and the secondly attack the surface with preference for sites of high energy (grain boundaries). As such this allows different crystal orientations, grain boundaries, precipitates, phase and defects to be distinguished easily during the observation stage. Always ensure that safety goggles are worn during etching to protect your eyes from coming into contact with the etchant. After etching, the specimen is rinsed in pure water and allowed to dry in air before observation. 5. Observation It is essential that the surface not be contaminated so as to maintain an accurate metallographic characterization for the specimen. As such ensure that surfaces are not touched (for e.g. by greasy fingers). Before observation, the specimen is mounted onto a glass slide with the use of a lump of plasticine and a levelling press. The levelling press is used to attach (compress) the specimen, plasticine and glass slide together and more importantly to ensure that the prepared surface is level. Also ensure that a piece of cloth is placed over the specimen surface to prevent contamination. Observation can commence by laying the specimen under a microscope. It is proper procedure to start the observation with the lowest magnification gradually up to higher magnifications to view the fine details. Focus the image by first using the coarse focus knob followed by the fine focus knob found on the optical microscope. For a more accurate assessment of the material, it is recommended that the specimen be examined before etching as some important features may be better visible at that stage and also that the specimen be examined at more than one site to achieve a more complete characterization of the specimens structure. Lastly, record these results by hand-sketch or by photographs.

4. Results & Discussion 4.1 Specimen X18 Details of material 0.8% carbon steel, heated for 1 hour at 800C, cooled in air, etched in Nital for 15 seconds

Sketch 1: Specimen X18 with 400x magnification Features observed The grains show a eutectoid microstructure across the specimen and is identified by the 2 phase lamellar arrangement of ferrite and cementite, which is also commonly called pearlite. Discussion of features The appearance of the eutectoid microstructure across the specimen can be explained by taking reference with the iron-carbon phase diagram. As specimen X18 contains 0.8% carbon, it hits the phase diagram at the eutectoid composition point therefore a lamellar structure is expected. As the specimen was heated for 1 hour at 800C this gave the material sufficient time for the austenite to evenly distribute across the microstructure. And as it underwent air-cooling, the austenite transformed into pearlite (combination of ferrite and cementite) when it crossed the eutectoid temperature of 723C. With the good distribution of austenite and generally slow air-cooling, it therefore gave the even distribution of lamellar pearlite.

4.2 Specimen X19 Details of material 0.35% carbon steel, cooled slowly from 870C, etched in Nital for 15 seconds

Sketch 2: Specimen X19 with 400x magnification Features observed The grains show a hypo-eutectoid microstructure as identified by the presence of 2 phases showing grains of ferrite and grains of pearlite. The pearlite phase shows a relatively darker appearance as compared to the lighter ferrite. The proportions of the 2 phases appear to approximately be equal at 50% each. Discussion of features The hypo-eutectoid microstructure can be explained as the specimen has a lower carbon content of 0.35% and with reference to the phase diagram shows its composition point towards the left of the eutectoid point. As explained through the phase diagram, the austenite at 870C cools and then crosses the phase line into the alpha and gamma (containing ferrite and austenite) region where the formation of ferrite emerges. As it cools the ferrite continues to form and the composition of austenite continuously changes until it reaches the eutectoid temperature of 723C where the remaining austenite transforms into pearlite. This explains the final microstructure where both grains of primary ferrite and secondary pearlite can be observed. With the use of the lever rule at the eutectoid temperature, the specimen shows an equal distance between the phase lines and therefore backs the approximately even distribution of the 2 phases of 50% each.

4.3 Specimen X20 Details of material 1.3% carbon steel, slowly cooled from 970C, etched in Nital for 15 seconds

Sketch 3: Specimen X20 with 400x magnification Features observed The grains show a hyper-eutectoid microstructure as identified by presence of 2 phases showing grains of cementite and grains of pearlite. Cementite gives a relatively lighter appearance as compared to the darker pearlite. The cementite shows to locate itself around the grain boundaries and approximately shows a 1015% proportion of the specimen. Discussion of features The hypo-eutectoid microstructure can be explained as the specimen has a higher carbon content of 1.3% and with reference to the phase diagram shows its composition point towards the right of the eutectoid point. As explained through the phase diagram, the austenite at 970C cools and then crosses the phase line into the gamma and Fe3C (containing austenite and cementite) region where the formation of cementite emerges. As it cools the cementite continues to form and the composition of austenite continuously changes until it reaches the eutectoid temperature of 723C where the remaining austenite transforms into pearlite. This explains the final microstructure where both grains of primary cementite and secondary pearlite can be observed. With the use of the lever rule at the eutectoid temperature, the specimen shows an proportion distance between the phase lines of about one tenth and therefore backs the approximate proportions of cementite and pearlite. The setback of this microstructure is that cementite locates itself around the grain boundaries of the pearlite. As cementite has hard and brittle properties, it acts as the weak link in the material reducing its tensile strength. However, this may increase the specimens strength and may be desirable for end-users based on their applications.

4.4 Specimen X34 Details of material 0.35% carbon steel, undergone hot rolling process, etched in Nital for 10 seconds

Image 1 and 2 : Specimen X34 with varying magnification Features observed This specimen shows hypo-eutectoid microstructure as identified by the presence of 2 phases showing grains of ferrite and grains of pearlite. As in specimen X19, ferrite appears lighter as compared to pearlite. The grains show traces of deformation and from far gives a fibrous texture appearance. Discussion of features As this specimen also contains 0.35% of carbon, the hypo-eutectoid microstructure is explained as per specimen X19. The difference with this specimen is that it has undergone hot working and therefore gives a different microstructure when compared to specimen X19. Although generally quite equiaxed, traces of deformation can be explained as the specimen underwent hot rolling. Hot rolling although deforms the material and microstructure in the process of working, it also introduces heat into the material at a specific critical temperature that allows the grains to recover and recrystallize back to its original shape, giving the specimen its features. In addition, the process of hot rolling where the microstructure is deformed and squeezed together causes banding and therefore gives the specimen its fibrous texture appearance. It is important to note that materials that have undergone banding show directional properties where properties are stronger along the direction of banding and are weaker perpendicular to this direction.

4.5 Specimen X31 Details of material 20% zinc brass, undergone hot extrusion followed by cold drawing, etched in alcoholic ferric chloride for 60 seconds

Image 3 and 4 : Specimen X31 Features observed The specimen shows a single-phase microstructure of alpha brass as referenced from the phase diagram. In far magnification, the presence of deformation and slip lines can be seen. The slip lines show a preference to run along 2 main directions perpendicular to each other. In close magnification, the presences of twins are observed. Discussion of features As mentioned earlier, with reference from the phase diagram this specimen with 20% of zinc only contains a single-phase microstructure of alpha brass. However the evidence of twins can be explained by it undergoing the process of hot extrusion where recrystallization took place. In the recrystallization process, some grains experienced growth symmetrically in the same lattice points and therefore had to reorganise its structure to a more stable state to co-exist giving the appearance of a pair of parallel lines across the grain. The subsequent cold drawing process the specimen underwent after hot extrusion can explain the appearance of the slip lines and slightly deformed grains. Through the process of cold drawing, the material was subject to plastic deformation and so called squeezing which resulted in the slipping motion of the crystal structure as well as its deformed grain appearance. The slip lines preferential direction was also due to the initial crystal structure of the specimen where its initial orientation created a more favourable direction for the grains to slip.

4.6 Specimen X32 Details of material 20% zinc brass, undergone hot extrusion followed by cold drawing and lastly annealed for 1 hour at 600C, etched in alcoholic ferric chloride for 60 seconds

Image 5 and 6: Specimen X32 Features observed The specimen shows a single-phase microstructure of alpha brass as referenced from the phase diagram. In far magnification, the microstructure generally shows even and non-deformed appearance. In close magnification, the presences of twins are also observed. Discussion of features As this specimen underwent the same processes as specimen X31 except for its additional annealing for 1 hour at 600C, certain features on its microstructure can be explained as per in the section 4.5 (specimen X31). The generally even and nondeformed appearance is the result of the annealing process, which allowed the material to reach a critical temperature to allow recovery and recrystallization. In the process of annealing, the introduced heat allowed the atoms to diffuse and re-grow therefore removing the slip lines that were seen in X31 and also allowed the grains to grow back into its non-deformed state giving the specimen its more even nondeformed appearance. The presence of twins were cause by hot extrusion process as well as the annealing process and their formation of parallel lines across the grains are explained as per section 4.5 (specimen X31).

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4.7 Specimen X33 Details of material 40% zinc brass, undergone hot extrusion followed by a moderate cold drawing process, etched in alcoholic ferric chloride for 10 seconds

Image 7 and 8: Specimen X33 Features observed The specimen shows a 2-phase microstructure of alpha and beta brass as identified by the phase diagram. Alpha brass gives a lighter appearance and the beta brass gives a darker appearance. In close magnification, the evidence of slip lines and twins can be seen in the alpha grains. In far magnification, the specimen gives a fibrous texture appearance as well as show elongated-grains. Discussion of features As mentioned above, with reference from the phase diagram this specimen with 40% of zinc contains a 2-phase microstructure of alpha brass and beta brass. The appearance of the slip lines can be explained by it undergoing the process of hot extrusion and cold drawing where the microstructure and grains were deformed/compressed to slip. The slip lines only appearing in the alpha brass grains can be possibly be explained by alpha brass being rather softer than beta brass (therefore deforms first) or simply due to dark appearance of beta phase that made identifying slip lines difficult. The process of hot extrusion can explain the appearance of the twins as per earlier brass specimens. The appearance of the fibrous texture and elongation of grains can be explained by compressive and deforming nature of both hot and cold working. In addition, the substantial difference in strength between the 2 phases allows for easy banding of the 2 phases aiding in its fibrous texture appearance.

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4.8 Specimen X Details of material etched in Nital for steels and etched in alcoholic ferric chloride for copper alloys

Sketch 4: Specimen X Features observed The specimen shows a 2-phase microstructure where one of the phases appears light with equiaxed grains and the other appears dark with elongated grains. The microstructure also shows ordered regular arrangement and shows an approximate proportion of the darker phase of about 10%. Discussion of features Since the microstructure shows a rather imbalance (1:10) proportion of the 2 phases and that the secondary phase does not form along the grain boundaries of the other phase, it can be predicted that this specimen is possibly a hypo-eutectoid steel specimen. With the ferrite grains as the lighter phase and the pearlite grains as the darker phase. By use of the lever rule, the composition of carbon can be predicted to be 0.02-0.03% to allow for a higher proportion of ferrite in the material. The equiaxed and orderly elongated grains of the 2 phases give an indication that some kind of heat treatment (for recrystallization) has been undergone as well as an indication that some rolling (deforming) process has been undergone too. To achieve this final microstructure, 2 possible routes of manufacture can be processed. First, a hot rolling process that combines cold working and annealing where heat allows recrystallization to form the equiaxed grains as well as deformation to create the elongated grain appearance simultaneously. Second, is a process of cold rolling followed by annealing as cold rolling would create the elongated grain appearance on pearlite and the subsequent process of annealing allowing recrystallization of the ferrite grains into its equiaxed shape.

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5. Conclusion Through this lab, two common metal alloys (steel and brass) that have high applicability in everyday engineering were studied and analysed at a microscopic level giving the students a better understanding and rationalisation of how microstructures affected the final materials property. It was also understood that there were factors such as the materials compositions, route of manufacturing and subsequent treatment it underwent that eventually gave the material its range of final properties. With this understanding, it allows students and engineers-to-be to predict the mechanical properties of a material upon seeing its microstructure, but more importantly allows students to be able to apply these concepts to choose the appropriate materials for engineering applications and for research and development of new materials. 6. References Steel Wikipedia, the free encyclopedia. 2012. Steel - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Steel. [Accessed 24 April 2012] Brass Wikipedia, the free encyclopedia. 2012. Brass - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Brass. [Accessed 24 April 2012] Work Hardening Wikipedia, the free encyclopedia. 2012. Work Hardening Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Work_hardening. [Accessed 24 April 2012] Dislocation Wikipedia, the free encyclopedia. 2012. Dislocation - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Dislocation. [Accessed 24 April 2012] Hall-Petch Relationship Wikipedia, the free encyclopedia. 2012. Hall-Petch Relationship - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Hall-Petch_relationship. [Accessed 24 April 2012] Grain Growth Wikipedia, the free encyclopedia. 2012. Grain Growth Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Grain_growth. [Accessed 24 April 2012] Annealing (metallurgy) Wikipedia, the free encyclopedia. 2012. Annealing (metallurgy) - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Annealing_(metallurgy). [Accessed 24 April 2012] Hot Working Wikipedia, the free encyclopedia. 2012. Hot Working - Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Hot_working. [Accessed 24 April 2012] Crystal Twinning Wikipedia, the free encyclopedia. 2012. Crystal Twinning Wikipedia, the free encyclopedia. [ONLINE] Available at: http://en.wikipedia.org/wiki/Crystal_twinning. [Accessed 24 April 2012]

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