This action might not be possible to undo. Are you sure you want to continue?
Assignment Cover Sheet: Academic Year 2012/2013
Date of Hand up: 25h April 2013
Course: ME in Mechanical Engineering Subject: Surface Engineering Title of Assignment:
Sample Preparation for Surface Engineering Microscopy Investigation
Name: Lannon Adamolekun
Student Number: C08753211
Lecturer: Dr. Gareth O’Donnell
This is most commonly done using a conventional light microscope. Structures which are coarse enough to be visible to the naked eye are termed macrostructures while those which require magnification to be visible are termed microstructures.TITLE: Sample Preparation for Surface Engineering Microscopy Investigation 1 INTRODUCTION The examination of materials by optical microscopy is essential in order to understand the relationship between properties and microstructure. The first step obviously is to cut the specimen to size and to grind and polish the surface to expose the feature(s) of interest. of course. the basic concern being that the specimen prepared be a true representative of the sample. However useful information can be gained by examination with the naked eye of the surface of metal objects or of polished and etched sections. and by proper selection of rotational speed. Sectioning is generally done by saw or cutting wheel and these wheels have counterbalanced loading to avoid excessive pressure on the sample. The size depends on the microscope and could range from a few centimetres. specimen preparation is crucial. Simultaneous lubrication and cooling with water. The preparation of a specimen to reveal its microstructure involves the following steps and each will be discussed briefly. or alcohol is desirable. oil. and saw . is that the specimen be cut to size. 2 Cutting a Specimen The most obvious requirement. Sectioning a sample to be examined – must be careful not to significantly alter the microstructure during sectioning Mounting in resins (if sample is too small) Coarse grinding and grinding on progressively finer emery paper Polishing using alumina powder or diamond paste on rotating wheel Etching in dilute acid (2% Nital for steel) Washing in Alcohol and drying Typical magnifications used are between 50x and 1000x For both optical and electron microscopy. cutting pressure.
There are many different cutting methods. compression molds. nd Dear all the following are guidelines for your 2 short report: The title of this report is “Sample Preparation for Surface Engineering Microscopy Investigation”. The mounting material used should not influence the specimen as a result of chemical reaction or mechanical stresses and it should adhere well to the specimen e.size. with surface damage extending to less than 1 mm. cold mounts and other choice of epoxies available. It also minimises the amount of damage likely to be caused to the specimen itself. although some are used only for specific specimen types. it is possible to get thin (perhaps 100 mm) slices of even the hardest materials.g. 3 Mounting Mounting of specimens is usually necessary to allow them to be handled easily. 4 Grinding After the sample has been sliced. the surface needs to be ground and polished to get a flat face with uniform analysis conditions across the region of interest 5 Polishing 6 Etching Sample preparation for solid surfaces and films Surface Engineering Lab Report. Cutting with abrasives may cause a large amount of damage. whilst the use of a low-speed diamond saw can cause fewer problems. .
Submit by 9pm. The amount of damage depends on the method by which the specimen is cut and the material itself. either in a thermosetting plastic (e. The variation in material properties will affect how the preparation should be handled. Mounting Mounting of specimens is usually necessary to allow them to be handled easily. acrylic resin). Specimens can be hot mounted (at around 200 °C) using a mounting press. thin V’s thick coated samples. chemical attack. Regards. for example very soft or ductile materials may be difficult to polish mechanically. Cutting with abrasives may cause a large amount of damage. Ensure that you mention what is being achieved by each step. although some are used only for specific specimen types. for example through heating. visit given a detailed account of each step. then the mounting material should also be electrically conducting. it is important to produce something that is representative of the whole specimen. All work must be the author’s own work. It is not always possible to achieve this with a single sample.g. 25 April by email. It also minimises the amount of damage likely to be caused to the specimen itself. The mounting material used should not influence the specimen as a result of chemical reaction or mechanical stresses. phenolic resin). or a thermosoftening plastic (e. or mechanical damage. Thursday.Based mainly of the information and equipment presented during our lab. Cutting a specimen It important to be alert to the fact that preparation of a specimen may change the microstructure of the material.g. ensuring that the coating stays intact during preparation. Indeed. it is always good practice to mount samples from a material under study in more than one orientation. if the specimen is to be electropolished (an Electrolytic process ) or examined under a Scanning Electron Microscope . whilst the use of a low-speed diamond saw can cause fewer problems.g. Include in this report considerations which should be made in designing preparation sequences for different types of samples. the equipment used and the precautions which need to be taken when preparing Surface Engineering Microscopy samples. e. Simple small hand-drawn diagrams can be included. If hot . a hard coating on a soft substrate. a soft coating on a hard substrate. There are many different cutting methods. etc. Mention is this reports some of the information which can be obtained from such investigation and both some of the functions and limitation of microscopy. Gareth th Sample Preparation for Surface Engineering Microscopy Investigation For Metals When preparing samples for microscopy. It should adhere well to the specimen and. This report may have a simple cover sheet and be no more than two pages of content only.
Typically. acrylic or polyester resin. The grinding procedure involves several stages. to prevent rocking during grinding and polishing. the specimen is thoroughly washed with water. the finest grade of paper used is the 1200. Between each grade the specimen is washed thoroughly with soapy water to prevent contamination from coarser grit present on the specimen surface. the coarsest grades of paper are often not useful. and to preserve the open structure of the material. Each grinding stage removes the scratches from the previous coarser paper. . It is possible to determine the start point for grinding using the following empirical relationship where the width of the largest scratch is measured under a microscope: This prevents putting more damage into the sample than already exists. and once the only scratches left on the specimen are from this grade. A mounted specimen usually has a thickness of about half its diameter. 180 grit paper is coarser than 1200. So. to prevent grit. The edges of the mounted specimen should be rounded to minimise the damage to grinding and polishing discs. The coarseness of the paper is indicated by a number: the number of grains of silicon carbide per square inch. for example wet silicon carbide paper. but is not essential. followed by alcohol and then allowed to dry. Cleaning specimens in an ultrasonic bath can also be helpful. The series of photos below shows the progression of the specimen when ground with progressively finer paper. Mounted specimens are ground with rotating discs of abrasive paper flushed with a suitable coolant to remove debris and heat. e.mounting will alter the structure of the specimen a cold-setting resin can be used. using a finer paper (higher number) for each successive stage.g. for example. A diagram of a mounted specimen Grinding Surface layers damaged by cutting must be removed by grinding. epoxy. polishing media or etchant being trapped in the pores. This is more easily achieved by orienting the specimen perpendicular to the previous scratches. and watching for these previously oriented scratches to be obliterated. Porous materials must be impregnated by resin before mounting or polishing.
typically with diamond particles 6 microns in diameter which should remove the scratches produced from the finest grinding stage. and a finer polish – typically with diamond particles 1 micron in diameter. Particles of two different grades are used : a coarser polish . to produce a smooth surface. Before using a finer polishing wheel the specimen should be washed thoroughly with warm soapy water followed by alcohol to prevent contamination of the disc.Copper specimen ground with 180 grit paper Copper specimen ground with 400 grit paper Copper specimen ground with 800 grit paper Copper specimen ground with 1200 grit paper Polishing Polishing discs are covered with soft cloth impregnated with abrasive diamond particles and an oily lubricant. .
but it is often hard to completely remove them all. such as boundaries and defects. highly deformed layer introduced during grinding and polishing. etching creates contrast between different regions through differences in topography or reflectivity. This means contrast may arise through different mechanisms – therefore revealing different features of the sample. It also removes the thin. etchants will preferentially attack high energy sites. Mechanical polishing will always leave a layer of disturbed material on the surface of the specimen. In alloys with more than one phase. the phase present and the stability of the region. The rate of etching is affected by crystallographic orientation. In all samples. if the specimen is particularly susceptible to mechanical damage (or excessive force is used in the grinding and polishing stages) debris can become embedded in the surface and plastic deformation may exist below the surface. Etching Etching is used to reveal the microstructure of the metal through selective chemical attack. leaving an undisturbed surface.Copper specimen polished to 6 micron level Copper specimen polished to 1 micron level. Electropolishing or chemical polishing can be used to remove this. . Ideally there should be no scatches after polishing.
for etching stainless steel or copper and its alloys. etched for too long. ie. This is applied using a cotton bud wiped over the surface a few times (Care should be taken not to over-etch . although it is important to remember what features you are trying to observe – repeatedly grinding a very thin sample may leave nothing to see. the photos below may be of some help). They may occur preferentially in regions of high local disorder.The specimen is etched using a reagent. . For example. containing a few drops of hydrochloric acid is used. The specimen should then immediately be washed in alcohol and dried. and obscure the main features to be observed. they do not represent features of the microstructure. in most cases.this is difficult to determine. a saturated aqueous solution of ferric chloride. If this occurs it may be better to grind away the poorly etched surface and re-polish and etch. These are etch pits caused by localised chemical attack and. however. these pits tend to grow. for example where there is a high concentrationof dislocations. Following the etching process there may be numerous small pits present on the surface. If the specimen is over etched.
making it level. the image will pass in and out of focus as the viewing area is moved across the surface. If it is not. it will make it difficult to have the whole of the field of view in focus . A small piece of paper or cloth covers the surface of the specimen to avoid scratching.Etched copper specimen Over etched copper specimen Ideally the surface to be examined optically should be flat and level. By using a specimen levelling press (shown below) this problem can be avoided. as it presses the mounted specimen into plasticene on a microscope slide. Specimen levelling press . In addition.while the centre is focused. the sides will be out of focus.