Mech1006 Materials & Mechanics

Laboratory Report Cover & Feedback Sheet Metallography & Microstructure: Lab Session M, 2013, Dr A Wojcik
Students must complete the top part of this sheet in block capitals (or typed). Student Name: Loc Nguyen Lab Group: 1

I confirm this report constitutes all my own work

SIGNED Loc Nguyen Please date stamp this sheet upon submission Degree Course: Mechanical Engineering Date of Lab Session 8/10/2013 Personal Tutor: Dr.Shipley

Due Date 5/11/2013 Received/Initials...........................................

(for Departments use)

Date Submitted......................................... Grading and Feedback (for Departments use)

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Presentation of report (structure, appearance) Language (grammar, spelling and punctuation) Quality of drawn microstructures Analysis and discussion of results Evidence of understanding of subject Answers to questions in lab script General comments

Grades A, B, C, D & E correspond broadly to First, Upper Second, Lower Second, Third and Pass degree standards respectively

Overall Grade ........................

Marked by Dr A Wojcik, 2013-2014 Department of Mechanical Engineering, University College London, WC1E 7JE

Content Page
1. Introduction/page 3 2. Theory/page 3-9
Structure of crystal Dendrites, grains and grain boundaries: Structure of alloys Sample preparation in metallography:

3. Results/page 9 -12 4. Discussions/page 12-16 a. Purpose of metallography: b. Idealised dendrite and the reason of the difference in X6, X7s dendrite to
c. the idealized version: Equiaxed grains vs. columnar grains in essentially same metals X1 and X1A Three forms of porosity Coring Eutectic structure Oil immersion can improves the resolutions of a lens

d. e.
f. g.

5. References/page 17 6. Sketches of each specimens/ page 18-19

1.Introduction
The following report will concentrate on optical microscopy, as well as the sample preparation required to evaluate microstructures. The optical microscopy testing on 7 different materials to evaluate the grain size, phases in specimens and composition inside the materials. From the observations, we can be able to determine different compositions, phases, deflects inside the materials and from that we can conclude what affect on them. Also to do the test, microscope also is learnt and discussed how to improve the resolution of the lens.

2. Theory Structure of crystals:

All matter is considered to be a mixture of chemical elements. These are the smallest units that are distinguishable on the basis of their chemical activity and physical properties. Inside the elements are atoms, which have a distinct structure characteristic of each element. Atoms are too small to be seen without the aid of ordinary microscopes. The mechanical properties of metals then derive from their crystalline structure. That is, the atoms in solid state of a metal are arranged in definite 3D geometric patterns to form crystals or grains of the metal. The network formed by joining the centre of the atoms in a crystal is called the lattice. The smallest volume in a lattice, which properly represents the position of the atoms with respect to each other, is known as the unit cell. There are 14 types of unit cells but the structures are common and can separated as following:

(a)

(b)

(c)

(a) Body-centred cubic (BCC); (b) Face-centred cubic (FCC); (c) Hexagonal closepacked (HCP) The alignment of the atoms has an important part in mechanical properties of metals. For example, BCC is strong structure, and in general, the metals that are hard and strong are in this form at normal temperature; FCC is characteristic of ductile metals and the metals with HCP structure are quite susceptible to work-hardening. 3

Dendrites, grains and grain boundaries:

When a metal is cooled from liquid state to solid state, because cooling cannot be exactly the same for every atom, certain atoms will be attracted to each other to form a unit cell ahead of others. This unit cell becomes the nucleus for crystal formation. During the solidifying, the nuclei keep growing and crystallising then form dendrite. The term dendrite comes from Greek word Dendron, which means a tree. This description is appropriate because we can describe the form and structure of a metallic dendrite as like a tree: With a main branch, from which grow side branches, from which grow smaller side branches, and so on, until all the main branches and the side branches grow into each other and there is no room for any more branches to grow then it form grains and keep growing. This orderly growth of the grain continues in all directions until it runs into interference from other grains that are forming simultaneously about other nuclei. Dendrite structure

How the dendrite forms and ideal dendrite structure

The process of the formation of grains and grains boundaries If two grains that have the same orientation meet, they will join and form a larger grain, but if they are forming about different axes, the last atoms to solidify between the growing grains will be attracted to each other and much assume compromise positions in an attempt to satisfy a double desire to join with each other. These misplaced atoms are in layers about the grains and are known as grain boundaries. They are interruptions in the orderly arrangement of the lattices and offer resistance to deformation of the metal. A fine-grained metal with a large number of interruptions will be harder and stronger than a coarse-grained metal of the same composition and condition. Polishing the metal specimen can sometimes reveal the grain structure but chemically etching the specimen, after polishing, dramatically enhances the appearances of the grain boundaries. Grain boundary in brass

Structure of alloys
Grains of a particular composition are referred to as being made from the same phase. A pure metal will cool to give single phase grains. An alloy is a substance that has metallic properties and is composed of two or more chemical elements, of which at least one is a metal. Most commercially used metallic materials are not pure metals but alloys, which consist of more than one elements. Some of them may be non-metallic elements. Fundamentally, there are modes of arrangement of atoms or phases exist in alloys. These phases are: pure metal, solid solution and compound. For simplicity of illustration, with 2 elements A and B, shall be considered in the following discussion: Pure metal: If there exist no B-atoms in A-crystal grains and no A-atoms in B-grains. Solid solution: Any solution is composed of two parts: a solute and a solvent. The solute is the minor part of the solution, which is dissolved, while the solvent constitutes the major portion of the solution. There exist B-atoms (solute) in A-crystal grain (solvent). Compounds: There are generally formed between chemically dissimilar metals and are combined by the following rules of chemical valence. Elements A and B form a compound AB but unlike solid solution, the ratio of the number of A-atoms to B-atoms is fixed (ex. 1:2).

Phase transformation can happen by both the concentration of the alloying elements and the temperature of the metal.

Copper and iron phases in a cold pressed metal.

To determine the phases inside the metals, we can use optical microscope experimentally on the metal but also can analysis theoretically from a composition/temperature map called as an equilibrium phase diagram. From the graph, we can identify the phases in metal at each different temperature and condition. However, to minimise error, we should also combine it with using microscope.

Fig 2.6: An example of equilibrium phase diagram

Sample preparation in metallography:

In order to identify and evaluate the microstructure of metals, it is very important to prepare the samples properly and with great care. The various steps in specimen preparation include: Selecting a representative sample of the materials to properly characterize the microstructure or the features of interest. This step is critical to the success of any subsequent study. The second, equally important step is to correctly prepare a metallographic specimen. Sectioning the sample carefully to avoid altering or destroying the structure of interest. The most widely used sectioning device is the abrasive cut-off machine, ranging from units using thin diamond-rimmed watering blades to those using wheels. To minimise burning and deformation, a lubricant or coolant is typically used. However no matter how carefully we sectioned the sample, a small amount of deformation occurs on the sample surface. This is reason we need to grind the sample later. Mounting the section without damage to the sample in a plastic or epoxy material to facilitate handling and the grinding and polishing steps. Because large specimens are generally more difficult to prepare more than small ones, specimen size should be minimised. Grinding to achieve a flat sample with a minimum amount of damage to the sample surface. Grinding is generally performed by the abrasion of the specimen surface against water-lubricated abrasive wheels. Grinding develops a flat surface with a minimum depth of deformed metal and 7

usually is accomplished by using progressively finer abrasive grits on the grinding wheels.

A layer of disturbed metal

A layer of disturbed metal is removed

Polishing the mounted and ground sample. Often automated, polishing can be performed by hand by holding specimen against a wheel, covered with a cloth pad impregnated with a polishing compound. Polishing should yield a scratch-free surface

Improper polishing vs. proper polishing Etching in the proper etchant to reveal the microstructural details such as grains, grain boundaries and phase boundaries. Various etching techniques are available which chemical and electrochemical attack are mostly used. Washing the specimen in water and examination under a microscope.

The microscope we use to investigate the metals is a reflected light microscope. It passes the visible light transmitted through of reflected from the sample through a

single or multiple lenses to allow a magnified view of the sample. The resulting image can be showed up directly to our eyes through eyepieces or captured digitally and put on a TV screen. To get a between view or to have bigger magnification, we can adjust the focus or change lenses. Before put the specimen inside the microscope, we need to secure it on a glass slide and avoid human contact unless fingerprint is the only thing we want to see. After that, starting with lowest option of the magnification so we can have better look of the whole structure of metals and change the focus if necessary to get a clear view. To minimise error, we also need to redo the experiment at different area of the specimen to ensure a whole structure of the specimen is seen.

3.Results
Following specimens are used in this experiment: X1 With bare eyes, we can see this specimen has relatively long, columnar grains radiating in toward the centre. The grains also have different degrees of brightness of light reflecting from the specimen when we move the object. It happens due to the light orientations into the specimen at different angles so we can see a brighter and darker part. This is a pure zinc ingot so there is only 1 phase, which is zinc. As mentioned above, the columnar grains radiate toward the centre of the specimen; it is because of the casting process. Since the casting process extracts heat from outside through walls of a mould, small equiaxed grains from at this stage at the outside edge of the ingot. As the solidification process happens, some of small grains, having favourable growth axis into the centre, start to grow in the direction opposite to the direction of heat flow. They extend more rapidly than the ones next to them and begin to take more places than the slower growing grains. This is why we have different length and width columnar grain structure toward the centre. X1A Different from the specimen X1, this is an impure zinc ingot that means there are two or more elements in the structure of specimen. With bare eyes, we can see an equiaxed grains structure and there is a little black dot in the centre of ingot. The equiaxed grains happen because X1A is an alloy and different elements inside the specimen can be the 9 X1 Pure zinc ingot. Sand cast, etched in hydrochloric acid, macro view X1A Zinc ingot as above but impure. Macro view, note central pore X2 Copper with 4% tin alloy, sand cast, etched in alcoholic ferric chloride. Dendritic structure may be cored. Micro view X3 Same as X2 but annealed for 2 hours at 700C, coring gone X5 Copper with 8.4% phosphorus alloy. Sand cast, etched in ferric chloride solution. Eutectic composition. Micro view X6 Same as X5 but 4.5% phosphorus. Hypoeutectic, with cored dendrites X7 As X5 but 10.5% phosphorus. Hypereutectic, with un-cored dendrites.

starting point for the grains to growth. So they growth at random points and various directions The black pore we see on top of the surface is due to pouring metal defects during the casting. X2

Microscopic examination at 50X shows a difference in shade of the grains giving us information that there are 2 elements in this material; and there are black lines as boundaries appearing. Moreover, a dark skeleton pattern will be observed inside the grains. This represents coring, or unevenness in the composition that is, in the present sample, variations of the tin content in the copper. X3

This specimen is similar to X2 except that there is no coring in the grains because the specimen was annealed at 700C for 2 hours. This proves that heating and let the material cool down for a specific time can help reduce the coring. We can also see there are lots of lines containing tiny black dots representing the porosity within the structure. X5

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Microscopic examination reveals that the grains are composed of colonies of fine eutectic structure, which contains two solid phases. These phases may have different crystal structures or the same crystal structure but different lattice. High magnification is required to show the structure more properly. There are evidences of cracks and black dots showing the effect of shrinkage deflects and evidences of porosity. Copper crystals (solid solution -phase) and crystals of copper-phosphide (Cu3P) have intergrown in an apparently lamellar pattern, which has tended to develop radially in each colony with often a coarsening of the structure at the boundaries. The -phase appears dark or brown as it is preferentially attacked by the etching solution. The Cu3P appears white. Occasionally, free pieces of either Cu3P or -phase may be seen. X6

As this alloy contains excess copper with respect to the eutectic composition, there are separate copper-rich crystals (-phase) together with the eutectic, which is distinctly

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coarser than that in X5. Further, the eutectic regions have a fringe of Cu3P around them. The -phase crystals contain a relatively small amount of phosphorous in solid solution. There are cored dendrite, and ranged in shade from dark to light brown. These crystals grew first in the melt and they have developed in a characteristic dendritic shape. In fact, the dendritic form is not well developed, the crystals being rather rounded and stubby. Some of the apparently isolated, round shapes probably represent regions where the micro-section has passed through a dendrite arm. As the illustration above, there is a huge black dot believed to be a void in the material. It is an evidence of porosity caused by the gas formation during casting. X7

In effect, the reverse of X6 in that rounded dendrites of Cu3P are set in the background of the eutectic. The dendrites (white in appearance) seem to be better developed than in X6. However the present dendrites are not cored. At higher magnification, we can see a large gas pore presenting deflects in casting.

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4. Discussion
a) Purpose of metallography: Metallography is the study of the microstructure of all types of metallic alloys by use of low-magnification, optical microscopy and scanning electron microscopy. It can be more precisely defined as the scientific discipline of observing and determining the chemical and atomic structure and spatial distribution of the constituents, inclusions or phases in metallic alloys. By extension, these same principles can be applied to the characterization of any material. Many important macroscopic properties of materials are highly sensitive to the microstructure. Critical mechanical properties, such as tensile strength or elongation, as well as other thermal or electrical properties, are directly related to the microstructure. The understanding of the relationship between the microstructure and macroscopic properties plays a key role in the development and manufacture of materials and is the ultimate aim of metallography. Metallography, as we know it today, owes much to the contributions of the 19th scientist Henry Clifton Sorby. His pioneering work with modern manufactured iron and steel in Sheffield (UK) highlighted this intimate bond between the microstructure and macroscopic properties. As he stated towards the end of his life: In those early days, if a railway accident had occurred and I had suggested that the company should take up a rail and have it examined with the microscope, I would have been looked upon as a fit man to send to an asylum. But that is what is now being done b) Idealised dendrite and the reason of the difference in X6, X7s dendrite to the idealized version:

Compared to idealised dendrite, the dendrites in X6 and X7 are rounded and stubby. It represents there may be micro-sections passing through the dendrite branches and making the arms not connect to each other. c) Equiaxed grains vs. columnar grains in essentially same metals X1 and X1A As mentioned above, X1 is a pure metal and X1A is impure so the equiaxed grains presence is because of different elements inside X1A alloy. During the solidification process, they can be starting points for the dendrites to growth with various directions at random points. So we can conclude that solid solutions have different grain structure compared to pure metal and phases in crystal have big impact on how the dendrite grow.

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d) Three forms of porosity From the illustrations, we can see there are three types of porosity, which are gas porosity, cracks and misruns: Gas porosity: Gas holes are spherical holes of varying size, usually fairly evenly distributed and formed by gas in the metal. The larger holes tend to be found in the heavier section. If the metal is correct prior to casting, the pinhole type of porosity is probably due to absorption of hydrogen from steam in the mould. As example, we can see lots of various sizes of black hole in the illustration of X5, X6 and X7 that are the results of gas porosity. Cracks: They are formed after the metal has become completely solid. Bad casting design that make contraction by the mould to the solid can create cracks. Also, X5 is an example for this. Misruns: It is a pouring metal defect occurring when the liquid of metal does not entirely fill up the mould, that leaving an unfilled volume. It is caused by lacking of fluidity in the molten metal. An example of it is a pore in X1A. e) Coring

Coring happens when a heated alloy cools in non-equilibrium conditions. As solidification proceeds, the compositions of the solid and melt must continuously adjust themselves in order to maintain thermodynamic equilibrium. This requires long-range diffusion of atoms within the solid and melt and exchange of atoms across the solid/melt interface, which will only occur if the system is cooled very slowly. If cooling is too fast, then there is insufficient time for diffusion to take place, resulting in the chemical unbalance in the growing crystals. This causes the exterior of the material to harden faster then the interior. Coring cause the centres of the grains to retrain more of the higher melting temperature element. In this case, the dendrite arms formed from the exterior have a different composition than the alloy in the inner regions, resulting in a local compositional difference. According to the coring definition, it suggests that coring creates the instability inside structure of material, which can lead to decreasing in some mechanical properties. As we know there is no coring happens in X3 because it is annealed for 2 hours, so we can 14

conclude to eliminate coring we need to maintain the thermodynamic equilibrium inside the specimen by annealing.

According to the equilibrium phase diagram above, we can determine how different compositions in metals affects the cooling or heating processes and solidification point of X6, X7 can also be found out by using diagram above. With those two specimens, they are both examples of hypoeutectic alloy. On slow cooling process, the liquid in X6 first solidifies at about 940oC as copper rich dendrites. The composition of the remaining liquid becomes increasing rich in phosphorus until it solidifies as a eutectic at the eutectic temperature of 714oC. However, with the X7 specimen, on the same slow cooling process, the liquid first solidifies as copper phosphide dendrites at approximately 850oC. The remaining liquid also solidifies as a eutectic at 714oC. The dendrites in X6 are cored, cause by non-equilibrium solidification: the cooling rate was too fast for equilibrium to be maintained between solid and liquid phases. However, there is no coring in X7s dendrites because of its narrow composition range. This result suggests that the difference in percentage composition can have a big impact on the pattern of dendrites. f) Eutectic alloys A eutectic-composition is an alloy of two or more metals, which will completely change from molten state to the solid at the same temperature. During heat-up, the eutectic composition will be the first to melt so it takes less energy during the process. 15

The silver-copper phase diagram h) Oil immersion can improves the resolutions of a lens In light microscopy, oil immersion is a technique used to increase the resolution of a microscope. This is achieved by immersing both the objective lens and the specimen in a transparent oil of high refractive index, thereby increasing the numerical aperture of the objective lens. The resolution of a microscope is defined as the minimum separation needed between two objects under examination in order for the microscope to discern them as separate objects. This minimum distance is label . If two objects are separated by a distance shorter than , they will appear as a single object in the microscope. A measure of the resolving power of a lens is given by its numerical aperture, NA:

Where is the wavelength of light, from this, It is clear that a good resolution (small ) is connected with a high numerical aperture. The numerical aperture of a lens is defined as:

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Where is the angle spanned by the objective lens seen from the sample, and n is the refractive index of the medium between the lens and specimen (=1 for air). Because sin is always less than or equal to unity, the NA can never be greater than unity for an objective lens in air. If the space between the objective lens and the specimen is filled with oil however, the NA can obtain values greater than unity. This is because oil has a refractive index greater than 1.

5. Reference
Liquid Penetrant and Magnetic particle Testing at level 2 by The International Atomic Energy Agency http://www.ami.ac.uk/courses/topics/0131_mb/ ME582 Laboratory Assignment and Individual Project Spring, Fall 2013 by Bill Warnes http://www.substech.com/dokuwiki/doku.php?id=solidification Materials and Minerals Science Course C: Microstructure http://www.facealuminium.com/ENG/Hot_topics/Techical_papers/Defects_of_diecast_ products2.asp Eutectics the good and the bad by Dan Kay http://pwatlas.mt.umist.ac.uk/internetmicroscope/micrographs/microstructures/mor e-metals/copper/phosphorus/10.5wt.html http://www.frankshospitalworkshop.com/equipment/documents/microscopes/wikip edia/Oil%20immersion.pdf Introduction to Metallography: www.metallographic.com http://www.labtesting.com/resources/testing-methods/metallography-andmicrostructural-evaluation/ http://www.leica-microsystems.com/science-lab/metallography-an-introduction/ Optical Metallography by Mr Louthan, Jr., Department of Materials Engineering, Virginia Polytechnic Institute and State University

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