METAL AND ALLOY (Experimental Guidance) PHY 4206 FZK 4206 Lecturer: Prof. Dr. Abd. Halim Shaari Demonstrator: Jabatan Fizik Universiti Putra Malaysia 43400 UPM Serdang Selangor DEREPORT WRITING Front cover Front page of reports should contain: Experiment Number, Experiment Title, Group Number, Group Members, Student Matrix Number and Date of Experiment Held. Introductions This section refers to the background and problems of experiment. Do mention the objectives of experiment. The aim of the experiment can be elaborate from the experiment objectives. Instrumentation ‘This section refers to the background and instrument used in the experiment. Experiments/Experimental Methods Reports procedure should be completed according to experimental guidance given. However, this section should be discussed in details for experiment which include instruments handling and computer software. If there are any changes in the experimental procedure, it should be mentioned in the report. Results and Analysis Date should be presented in table form or graphs. Certain parameters should be taken into account during analysis. Attention 1. Calculate the errors and uncertainties of reading taken in the experiment. 2. All calculations should be in SI units. 3. All graphs should be entitled and labelled according to its units. 4, Any formula or equation used in calculations should be written in the reports. 5. Define the symbols used in the experiment. Discussions Discuss the results gain from experiment. The discussion should be supported by the theories and references. Problems occur during the experiment which Influence results and suggestion are written down in this section. Conclusion Discussion should be simple and strong referring to the results and discussions section References ‘At least 3 references needed in order to fulfil the understanding of experimental. ‘Appendices should be attached as the last section of reports, Attention Reports should be submitted on the second week from the experimental heid.EXPERIMENT 1 MICROSTRUCTURE OBSERVATION 1, OBJECTIVES a. To develop skills on grinding, polishing and etching samples (ceramic and polymer) and observe samples microstructures using optical metallurgy microscope b. To understand basic principle of optical microscope and its utilities. c. To develop skills using Inverted Trinocular Microscope (VBT-2T). 2. AIMS a. To prepare sample holder. b. Able to observe microstructures on given specimens (ceramic and polymer), c. To compare photomicrograph before and after etching. 3. INTRODUCTION Materials microstructure consists of grain, grain boundaries, sediment, porosity, impurities and infinitesimal solution phase that can only be viewed using metallurgy microscope. Microstructure analysis is a structure characterization research of materials which correlate with mechanical properties and material physics. Microstructure is a characteristic that can be observes using optical metallurgy microscope after the precise sample preparation had taken place. Microstructure failures such voids and cleavage could be observed after the polishing process. However, for materials such metals and alloys, microstructures such as grain boundaries, alloy phases and surface layers can bee seen after the etching process. Microstructures observation techniques are useful and can be applied in: + Industrial; in metallurgy, alloy and ceramic quality assurance. * Advance materials research laboratory; in searching for new materials.There are few steps in microstructure analysis: 3.1 Sample holder Sample holder is made in order to hold the sample while doing other processes such as grinding and polishing There are two ways of preparing the sample holder: * Cold method ~ the mixture of epoxy and hardener is poured into a mold that contains the sample until the mixture become hard. + Heat method - sample is position in a hot compressor mold and being poured with fenolic substance. Then it is heated to certain temperature and compressed. Finally, the sample will stick to the pallet caused by compression given. 3.2 Sample cutting High-speed diamond cutter machine is used for cutting the sample surface. In cutting process, sample’s surface must be assured is free from anyyig scar. While cutting, the sample must be kept in moderate temperature using cooling liquid to: + Prevent deformation as the temperature arises while cutting. + Remove impurities at surface while cutting. 3.3 Grinding and Polishing 3.3.1 Grinding This process is done in order to remove the deformation and being used together with water to control the temperature of samples besides removing the balance of impurities. The grinding process is normally started with rough grinding using silicon carbide paper, size 80 or 120 mesh, which means that the roughness of the paper is about 500-10 micron Then, it Is followed by soft grinding using silicone carbide paper of 240, 320, 400 and 600 that give the surface’s roughness of 10-0.1 micron.3.3.2 Polishing After grinding, the sample is being washed and dried. Then, the sample needs to be polished using polishing machine to remove the deformation effect of grinding. Polishing machine contains soft fabric (silk, nylon and cotton). A diamond polisher material must be put onto the polisher board and the normal size of diamond polisher’s grains used are 6, 3, 1 micron 3.4 Etching Etching is done to get the surface structure of the sample. Normally, there are two ways of etching: * Chemical etching - etching process that use chemical liquid with the sample. * Thermal etching ~ etching process which heating up sample to a certain temperature. 3.5 Metallurgy microscope This microscope is using optical light reflection that contains: * Torching system, * Objective system, * Eye lenses microscope system. 4, MATERIALS AND APPARATUS. Diamond cutter machine Hand grinder machine Polishing machine Silicone carbide paper (600, 800 and 1200 mesh) Diamond polisher (6 and 1 micron) Metallurgy microscope Sample (metal, alloy and ceramic)5. EXPERIMENTAL PROCEDURES 5.1 Sample holder preparation a) Release agent being swept to the inner surface of mould and left dried. b) Placed sample into the mould. If the sample is pallet figure, it is placed vertically in the mould. 5.2 Sample cutting a) Dry samples are being sliced using machine with diamond biades. b) Coolants liquids are used in the cutting machine in order to prevent the deformation caused by the temperature, which increases while cutting process held. ¢) Samples that have been cut are washed with distilled water and left dried. d) The surface structures of samples after the cutting process are analyzed using the metallurgy microscope. 5.3 Grinding and polishing a) Grinding process is done using silicone carbide paper in order to remove the cutting deformation marks, b) The grinding process starts using low mesh value of silicone carbide paper (rough grinding) around 80 to 120 mesh and followed with fine grinding using silicone carbide paper (240, 320, 400 and 600 mesh). While grinding, a little amount of water is used in order to lower the temperature and to flow off grinding leftover. c) The samples are rubs onto the silicone carbide in vertical direction with rotations about 45° to 90° for about 2 minutes, as to get flat surface of samples. d) Samples are washed using distilled water and acetone after the grinding process and left dried. €) Polishing process is done using polishing machine in order to vanish the deformation marks occur during grinding processes. f) Diamond polisher with size of 6 micron is sprayed onto the polishing cloth (silk, nylon and wools) on the polishing plate and let it rotate for a while. g) Samples are placed onto polishing plate while push it firmly in the anti-clockwise direction. These steps are done for about 2 minutes.h) Steps g) are repeated using diamond polisher with size of 1 micron. ') Samples are washed using acetone and left dried. J) The samples analyzed using metallurgy microscope after polishing processes. This is done with cautious as to get the accurate surface image of the samples. 5.4 Etching @) Etching process depends on type of samples used. i, Ceramic Thermal etching is performed to ceramics samples at temperature less than 100°C (from samples sintering temperature) fer about 1 hour. ji. Metal or alloy Chemical etching is performed. The samples are dipped into 2% nitric acid solution for about 2-3 seconds. Nitric acid is an etching reagent. Then the samples are rinsed using distilled water and acetone and left dried. % ii, Sample’s miceBtEructu is observed after etching iv. If the microstructure observation is not clear, the etching process is repeated. Prepared by: Examined by (Mr Iskandar Shahrim Mustafa) (Prof Dr Abd. Halim Shaari)EXPERIMENT 2 EFFECT OF HEAT TREATMENT ON THE MICROSTRUCTURE 1. OBJECTIVES a. To determine the changes of nicrostructure of the samples (metals and alloys) due to the different types of heat treatment. b. To study the grain structures using metallurgy microscope. ¢. To study the effect of etching on the microstructure 2. INTRODUCTION The properties of metal and alloy can be ctianged by applying the heat treatment process. In this experiment, the technique that are will be used are annealing, normalizing and quenching 24 Annealing A term denoting a treatment, consisting of heating to and holding at a suitable temperature, followed by cooling at a suitable rate, used primarily to soften, but also to simultaneously produce desired changes in other properties or in microstructure. The purpose of such changes may be, but is not confined to, improvement of machinability; ation of cold working; improvement of mechanical or al properties; or increase in stability of dimensions, The time-temperature cycles used vary widely both in maximum temperature attained and in cooling rate employed, depending on the compcsition of the material, its condition, and the results desired There are 3 main steps of this process: + Heating the metals and alloys in certain temperature + Maintaining the temperature of the material in certain time for some changing to appear. * Slowly cooling, for example, in the furnace with the power supply switch off or caoling in the atmosphere or normalizing in the room temperature.2.2 Quenching + Rapid cooling:of metals and alloys in order to obtain desired properties; most commonly accomplished by immetsing the metat in oil, liquid nitrogen, salt or water. In the case of most copper base alloys, quenching has no effect other than to hasten cooling. In steel, the heat is used to produce the martensite steel. 2.3 Normalizing Normalizing is a process in which an iron-base alloy is heated to a temperature above the transformation range and subsequently cooled in still air at room temperature. 3 MATERIALS AND APPARATUS Furnace Mild Stee! (Keluli lembut) Metallurgy microscope Cooling medium Grinding and polishing Nitric acid (farutan nital) 4, EXPERIMENTAL PROCEDURES @) Heat 4 pieces of mild steel in the furnace at a temperature of 700 °C for 2 hours. b) Cool the first piece of mild steel in the furnace (annealing Process) and the second piece of mild steel at room temperature (normalizing process). ¢) Quench the third piece of mild steel in water and the last piece in oil. 4) Grind and polish all the specimens. e) Etch all the specimens using nitric acid and observe the microstructure on the surface for each specimens using microscope metallurgy Note: Refer lab manual 1 for grinding, polishing and etching process,5. QUESTIONS 1. Determine the microstructure and state the magnification of the samples for each heat treatment. 2. Compare the microstructure of all the samples for different types of heat treatment. 3. Discuss the microstructure of the samples from the aspect of the rate of cooling. 4. What Is the effect of different cooling rate on the microstructure of steel? 5. Clarify the factors that influence the changes in the microstructure of the steel 6. Clarify the uses of cooling process from the aspect of heat treatment in manufacture sector. Prepared by: Examined by: (Mrs Masrianis Bt Ahmad) (Prof Dr Abd. Halim Shaari)EXPERIMENT 3 MATERIAL'S HARDNESS TEST OBJECTIVES * To study basics operation technique of Rockwell hardness test machine, * To run materials hardness test based on Rockwell hardness scales. AIMS + To determine the average value of hardness for ceramic and polymer samples, INTRODUCTIONS Hardness is tested based on Ggficuity shown by materials upon ti locality deform such as indentat ‘and abrasion. Hardness test can be divided into 3 categories: @) Elastic hardness In elastic hardness case, the hardness can be measured using Scleroscope test. This test is used for rubber-based materiai, which the hardness value of materials is measured upon the depth increment of the indent inside the material. b) Abrasion hardness Abrasion hardness is determined using Mohr Skil and file test. Brittle minerals and materials are suitable for this test. In this experiment, tested materials will be scraped away with a known hardness scale mineral. c) Indentation hardness Indentation hardness is determined using several test method Such as Vickers, Brinell, Rockwell and Tukon (micro-hardness) Hardness test have been widely used in material testing and engineering field. Indenter is used to give force on specimenSurface. Stiff indenters with different geometrical shapes are Pressed on the surface of metal; polymer or other materials, which have plastic behaviour, and the indents sizes occur are measured. Hardness (H) is load rate, which is used onto indent area, occurred: Hardness (H) = Load/Indent area Hardness is mention in number form, which is disproportional with indent depth for several load and indenter or proportional with average load under indentation area, Rockwell hardness testing machine is a machine, which can read straight from scales or screen. An indenter is pressed onto a tested specimen surface. A calibrated dial shows indent increment, which is suitable with material hardness. The dial divided into 100 parts. A small reading shows a deep indention or low hardness and vice versa. The usual indenters used are diamond and steel ball with diameters 1/8 inch and 1/16 inch. Several loads are used in order to gain indentiog: dgpth not more than 0.2 mm or 100 parts. Herewith, Rockwelf#hardness numbers are divided into scales which are A, B, C, D, E, F G, H, and K where dependable to type of indent and load used (refer Figure 1) : Scale | indenter | Load A 60 |_ 220% D_ | DIAMOND |~100 C 150 E BALL £0 8 me 100] G 150 r H BALL }—80_| \ 1/8" 100 wP K 150] Ho. sa | | o 1a" 100 | { P [150] i £ Ba | 89 1/2" 100 V "(7150 Figure 1: Rockwell hardness test; indent type and test scales4. 5. MATERIALS AND APPARATUS * Digital Hardness Testing Machine (Twin Type) - Mitutoyo (ATK-600) * Specimens * Diamond indenter * Ball indenter 1/16” EXPERIMENTAL PROCEDURES a) Choose a suitable indenter according to the specimen and placed it onto the indenter holder. b) Placed the specimen on the anvil ¢) Set up the test parameter according to the hardness scales. d) Raised the sample on anvil until the reading on the screen appears and the LED stop blinking, e) Press START button, and the indenter will gradually move downwards and préSsing the. sample surface. The value for sample hardness will appear*8fter awhile. Jot down the value appears based on the hardness scales used, f) Take at least 6 sets of reading and average value for sample hardness. g) Repeat steps (a) until (f) for different samples. hh) Discuss the hardness differences between all the tested samples. States the reasons or factors, which caused the sample to be harden than the other samples. a6. QUESTIONS a) Explain the relation between hardness and stiffness on materials. b) State down several factors that causing hardness differences ‘on the same surface of any material. ) Gives the advantages of Rockwell hardness testing machine. Prepared by: Examined by: (Mr Iskandar Shahrim Mustafa) (Prof Dr Abd. Halim Shaari)Se ee eee EXPERIMENT 4 X-RAYS DIFFRACTION TECHNIQUE 1. OBJECTIVES * To understand the basic principles and instrumentation in X-ray diffraction * To investigate the use of XRD techniques in detection of elements. 2. AIMS * To determine the crystallographic structure of element, lattice constant and to identify the element. 3. INTRODUCTION X-ray can be scattered, diffracted and passed through a material, By assuming the lines of Ri, Ro and R3 in Figure 1 stands for a series of atom phases that parallel to crystal structure and separated each other at distance, d. ‘igure 1: X-ray diffraction by atoms Rx, Rz and Rs that separated at the distance, d.AB and AB’ represented X-ray lines with wavelength, A, and degree between phases, 8, going to phase and diffracted to BC and B’C’. Both waves are at the same phase and multiplications of the circle wavelength are: (A’B! + BIC!) - (AB + BC) = nA Bragg equation 1 2dsin @= nd When DB! = BYE = d sin @ ; @ = degree of Bragg Ba Powder Diffraction Method This method set the X-ray wavelength to be constant but change the degree of Bragg. The schematic figure for basic geometry of X-ray diffraction is as shown in Figure 2. Xray QQ” Ze er Powder sample Figure 2: Schematic figure of powder diffraction 4. MATERIALS AND APPARATUS. + Sampies are in powder or pallet type. * X-ray diffraction machine * X-ray source (target material: Cuprum, Cu). The X-ra monochrome used is CuK, type with wavenumber 1.54 A (1.5 x 107° cm). «Automatic graph recorder. 5. EXPERIMENTAL PROCEDURES. hya) Sample (powder or paliet) is inserted in the sample holder and the sample surface should be flattening in order to get a good reading. b) Placed the sample holder in the shutter. (Refer to the demonstrator or science officer for further details on machine operating technique) ©) Switch on the shutter and machine detector at the same time. d) Set the shutter at 80° rotation with starting rotation of 28=10°. (For further information on operating the computer's software of X-ray diffraction machine, refer to the operation procedures attached in the appendices in this experiment) e) Follow the safety precaution on radiation given by the science officer or demonstrator in charge. (General safety precaution in the XRD room is attached in the appendices) f) Determine the hkl value from the data obtain. 26 Ir T_d(ay Aki [ S=(h?+k?417)*7?] i | T 1 I | LO | Where, s=crystalline structure formulee 6. QUESTIONS Prepared by: Examined by a) Determine the compositions and structure formed by the samples, b) Determine the lattice parameter, a. (Mr Iskandar Shahrim Mustafa) (Frof Dr Abd. Halim Shaari)LAMPIRAN 1 Safety precaution in the XRD room 1. Switch ON the Air-con early morning for about 10 minutes before turning ‘ON any other equipment. (for first user) 2, Switch ON the chiller for about 5 minutes before switching ON X'pertAPD. 3. Make sure all equipment are ON by strictly following the sequent. 4, Always shut off (close) the shutter when each scanning is completed. 5, During the changing of the following sample, reduce the mA and follow by the k¥ slowly and OFF the HT power. 6. After each scan, stop for about 5 minutes for the system to cool down. 7. When finished using the X'pertAPD, make sure all the equipment is OFF before leaving the room. 8, Always keep the room cool, don't change the setting of air-con sciting to high temperature. 9. Don't bring in any diskette from outside of this room. 10. Always keep the room clean. 11, All the user must record some information (no.sample scan, time, date...) in the tog bocLAMPIRAN 2 Pi jure to on rtsw_software 1) "Power on” Monitor and Computer. © Wait until it's fully initilized . * Press the "ESC" key, as soon as pop out windows ask for User/Password 2) Double click X'pertsw Icon to start the X'pertsw software . ‘* Click on "X'pert organiser”and key in User name ~ XXXXX and Password = XXXXX with X'pert system. 3) Collecting Data Select module Click on "Data collector” to start routine measurement. click the "control" at the tool bar to link the computer with the X'pertAPD (online). press 0.k and close the pop out windows. press the "No" selection when the pop out windows ask for working offline. click the "measure" at the tool ber and click on "Program...", Select the scanning program that going to perform. key in the file name and the command for the scan. press O.K when everything had been key in. when the pop out windows shows "make sure the shutter is open" , press O.K. (Note : At this step the shutter should be open). Xpert APD now is doing the scaning. ‘+ After each scan, the data will be automatically save in the computer. ‘Remember to close the shutter, reduce the kV & mA in seqnent and then off the HV po 4) Process and analyse the scanning data * Select module Click on "Graphics and Identify" to start peak search and display the sea graph. Click "File" on the too! bar and press "new graph” to select the scaning graph. To print the display graph, click "File" on the tool bar and press “print” At the pop out window, tick the "hard copy of graph" at the graph sector and press O.1 To save the row data (txt file), click "File" on the tool bar and press "print". At the pop out window, tick the "texture report" at the pattern scctor and at the report select "x-y table” and then press O.K A windows will pop out to ask the destination of the output, select text file and then pres Select the destination (to hard disk or floppy disk) of the folder and press O.K to save the file, To search the scanning peak, click "Analyse" on the tool bar aad press "peak search’, Click 0.K at the pop out windows To print the peak list, click print, a pop out windows is display to ask for the destination. 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OBJECTIVES a) To understand the basic principles and instrumentation of dilatometer. b) To understand the use of dilatometer technique in determine thermal expansion coefficient. 2. AIMS * To determine samples elongation and thermal expansion coefficient. 3, INTRODUCTIONS Most of the material expanse when the temperature given increases. For 2 solid material, the expansion occurs in all direction at certain temperature. On contrary, if a thin metal rod is heated, the expansion is said to be happen in one direction. The infinitesimal change of length due to the change of temperature is defined by: Ad = kadT a) where /p the length at the reference temperature, To, and a is the linear thermal expansion coefficient. From equation (1) it follows that: (2) and a is generally a function of temperature, a = a(T). Assuming /o = constant, we obtain another useful relationship from equation (2): alii) _ de. a a (3) where ¢ is the relative elongation, «= ¢(7) Integrating equation (3) we gained:a(t) = falrar (4) In small temperature intervals, where7 — 7,, we can assume a = &% = constant (s) and (6) T-T, and ao can be calculated from a single experiment consisting of heating the sample from the initial temperature, To, to the final temperature, T, and measuring the relative elongation, «. While for volume expansion coefficient (f) is being recognized in the same way, where it is the ratio of changing in volume against changing in temperature at a constant pressure: av Oar (7) where #=3a 4, MATERIALS AND APPARATUS Dilatometer Forceps Micrometer screw gauge Samples 5. EXPERIMENTAL PROCEDURES @) The length of sample, /o is measured. b) The experiment undergo according the manual that given i. Switch on the amplifier, power supply and computer (approximately for 30 minutes before experiment). ll, Removes ceramic plug in the right opening of the furnace. Mi, Open the clamp and move furnace with protection tube to the right sideiv. Move the piston to the left side by pressing the dilatometer amplifier to the left side ATTENTION: Do not press right side as this will destroy the quartz system. v. Insert the sample in-dilatometer sample holder. vi. Move piston to the sample by pressing the button of the amplifier to the right side until piston and sample touches the key (sample is hold). ji. Start the dilatometer measurement software. Select from the main menu. * Program heating rate, dwell time, cooling rate ix, Check for the furnace temperature (should be below 30 °C). x. Now program the measurement. * Select , Type SAMPLE MEASUREMENT, + Select , setting. xi. Type in all sample information for the experiment. * Program SAMPLE FILE NAME- to store the data on the hard disk. * Select the ZERO FILE which should be used in the evaluation as default, + Program the END TEMPERATURE and DURATION (check also with the controller program, temperature profile and graphic). + Program the length of the sample and the measurement range. + Set the sarne range at the amplifier with digital switch * Select ; ; + Press to start auto zero detection. xii, Close the furnace with protection tube carefully so that sample does not shift. xiii. Lock furnace in the position of the left stop. xiv. Slide quartz tube out of the furnace and over the measuring system carefully. xv. Clamp protection tube, xvi. Insert ceramic plug into the right opening of the furnace. xvii, Start the measurement with xvili. Graph of Al(um) vs ATCC) are plotted and analyzed. ag6. QUESTIONS a) Assume that the sample is being used in gas pipe processing. The length of the pipes is 10 meters (2 = 20 cm’) and connected at temperature of 25 °C. The temperature of the pipes Increase up to 180 °C when used. Calculated the total length with the temperature changes and percentage of the pipes elongation when used. b) Based on question 1, assume that’ the pipes are rigidly connected between the two concrete in order to stop any elongation of the pipes. Calculate the pipes strain with changes in temperatures and force that impose onto the concrete. (given: total pressure = 29 x 10° psi) ©) Is it true that the thermal expansion coefficient has a constant value? State the reasons. 4) Thermal expansion is very: important for. certain material in Industrial processing especially the metal, why? Gives an example of related Industries. Prepared by: zi Examined by: (Mr Iskandar Shahrim Mustafa) (Prof Dr Abd. Halim Shaari) aa