Course No:

Experiment No:

Name of the experiment:

STRUCTURAL STUDY OF MILD STEEL AFTER HEAT TREATMENT

Date of Performance: Date of Submission:

Name: Reg. No: Session: Group:

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NAME OF THE EXPERIMENT:

STRUCTURAL STUDY OF MILD STEEL

AFTER HEAT TREATMENT

OBJECTS OF STUDY
Getting introduced to HEAT TREATMENT. To study structures of mild steel after heat treatment. Learning different microstructures that are produced after heat treatment. To produce a flat, scratch-free, mirror like surface.

INTRODUCTION
The definition of heat treatment of steel given in the handbook of metal is as A combination of heating and cooling operations timed and applied to a metal or alloy in the solid state in a way that will produce desired properties.

All heat treatment process involves the transformation or decomposition of austenite. 1. Metallography or microscopy consists of the microscopic study of the structural characteristics of a metal or an alloy. The microscope is by far the most important tool of the metallurgist from both the scientific and technical standpoints. It is possible to determine grain size and the size, shape, and distribution of various phases and inclusions which have a great effect on the mechanical properties of the metal. The microstructure will reveal the mechanical and thermal treatment of the metal, and it may be possible to predict its expected behavior under a given set of conditions.

The procedures and steps of heat treatment will be discussed briefly in the report:

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PROCEDURE HEAT TREATMENT PROCESS:

Fig. Exploded view of electric furnace used for heat-treating. Electric Furnaces Electric furnaces with a controlled atmosphere are frequently used for heat-treating on repair ships and tenders. Quite often two such units are used on the same ship. One is a relatively low-temperature furnace used for preheating or tempering, and the other is a higher temperature furnace used for hardening. Both types are equipped with control devices for regulating temperature. The high-temperature furnace may also be equipped with rheostats used to increase the rate of heating. An exploded view of a slightly The outer casing of the furnace is usually made of sheet steel. Just inside the casing is a layer of insulating material, such as mica, spun glass, or asbestos. Inside this insulating material is a lining of refractory material, such as firebrick and insulating brick. The refractory lining insulates the furnace, helps maintain the required high temperatures, and supports the heating elements and the hearth plate. Hearth plates are placed on the bottom of the heating chamber to support the pieces being heated. Hearth plates must withstand high temperatures without sagging or scaling. They are often made of a special nickel-chromium, heat-resistant alloy. If the furnace is designed for the heat treatment of high-speed steels, the hearth plate may be made of a carbon and silicon. Grids, usually made of iron-chromium-nickel alloy, keep heavy or long sections of material off the hearth plate. The use of grids ensures more uniform heating of the material and tends to prevent warping.

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COOLING EQUIPMENT The rate of cooling is controlled by selecting an appropriate cooling medium and cooling procedure. The equipment required for cooling includes the substances used for cooling, a tank or other container to hold the cooling medium, and various kinds of tongs, baskets, and other devices for handling and holding the work. The rate at which a metal cools depends upon a number of factors. The size, shape, temperature, and composition of the material and the temperature and composition of the cooling medium are the major Factors involved. The rate at which a cooling medium can absorb heat is also greatly influenced by circulation. When the cooling medium is agitated, the rate of cooling is much faster than when the cooling medium is not in motion. The volume of the cooling medium is also important. As the metal cools, the cooling medium absorbs heat. If the volume is insufficient, the cooling medium will become too hot to cool the work at the Required rate. In regular heat-treating shops where the cooling mediums must be used continuously, mechanical cooling systems are used to maintain the cooling medium at the correct temperature. Liquids, gases, and solids are all used as cooling mediums for heattreating operations. Solid materials such as lime, sand, ashes, and cast-iron chips are sometimes used when the rate of cooling must be slower than that produced by liquids or gases. We have used water as our quenching medium in the hardening process.

Figure. Portable quenching tank for use in heat-treating.

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TRANSFORMATION TEMPERATURES The first arrest at 2,800F marks the temperature at which the iron freezes. The other arrests (known as transformation temperatures or critical points) mark temperatures at which certain internal changes take place in the solid iron. Some of these temperatures are very important in the heat treatment of steel. As was mentioned before, the atoms in all solid metals are arranged in a definite geometric pattern. The atoms in iron immediately after freezing are arranged in the body-centered cubic structure. In this crystal structure the unit cell consists of a cube with an iron atom at each of the eight comers and another in the center. Each of the many individual grains (crystals) of which the solid metal is composed is built up of a very large number of these unit cells, all oriented alike in the same grain. This high-temperature iron is known as delta iron. At 2,550F, iron undergoes an allotropic transformation; that is, the arrangement of the atoms in the crystal changes. The new crystal structure is face-centered cubic, and the unit cell again consists of a cube with an iron atom at each of the eight corners, but with an iron atom in the center of each of the six faces instead on one in the center of the cube. This form is known as gamma iron. At 1,670F, iron undergoes another allotropic transformation and reverts to the body-centered cubic system. This structure, which is basically the same as the structure of delta iron, is stable at all temperatures below the A3 point and is known as alpha iron. The arrest at 1,420F is not caused by an allotropic change. It marks the temperature at which iron becomes ferromagnetic and is, therefore, termed the magnetic transition. Above this temperature iron is nonmagnetic.

Figure. Iron-carbon phase diagram.

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ANNNEALING: (EXPERIMENT PERFORMED BY OUR GROUP) ANNEALING is a term used to describe any heat treatment process that is used for the primary purpose of softening the metal. Two types of annealing processes are commonly used. FULL ANNEALING is done to soften the metal and make it more ductile, and to relieve internal stresses caused by previous treatment such as casting, cold working, or hot working. The operation known as PROCESS ANNEALING or STRESS RELIEF ANNEALING is done to soften the metal somewhat, although not as much as by full annealing, and to relieve internal stresses. In general, full annealing requires higher temperatures, longer soaking time, and slower cooling than process annealing. In the full annealing of steels, the steel is heated to a temperature that is 25 to 50F above the upper transformation point. In the process annealing of steels, lower temperatures are generally used. The rate of cooling used for annealing varies greatly, depending upon the metal being annealed and the degree of softening required.

Physical properties: Annealed metals are relatively soft and can be cut and shaped more easily. They bend easily when pressure is applied. As a rule they are heated and allowed to cool slowly. The animation above shows that an annealed metal is usually softer and can be deformed more easily than metals that are not annealed.

NORMALIZING:
It is held at this temperature to fully convert the structure into Austenite, and then removed from the furnace and cooled at room temperature under natural convection. This results in a grain structure of fine Pearlite with excess of Ferrite or Cementite. The resulting material is soft; the degree of softness depends on the actual ambient conditions of cooling. This process is considerably cheaper than full annealing since there is not the added cost of controlled furnace cooling. The main difference between full annealing and normalizing is that fully annealed parts are uniform in softness (and machinablilty) throughout the entire part; since the entire part is exposed to the controlled furnace cooling. In the case of the normalized part, depending on the part geometry, the cooling is non-uniform resulting in non-uniform material properties across the part. This may not be desirable if further machining is desired, since it makes the machining job somewhat unpredictable. In such a case it is better to do full annealing.

HARDENING:
Martensitic stainless steels are hardened by austenitising, quenching and tempering much like low alloy steels. Austenitising temperatures normally are 980 to 1010C, well above the

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critical temperature. As-quenched hardness increases with austenitising temperature to about 980C and then decreases due to retention of austenite. For some grades the optimum austenitising temperature may depend on the subsequent tempering temperature. Preheating before austenitising is recommended to prevent cracking in high-carbon types and in intricate sections of low-carbon types. Preheating at 790C and then heating to the austenitising temperature is the most common practice.

COOLING AND QUENCHING:

Martensitic stainless steels have high hardenability because of their high alloy content. Air cooling from the austenitising temperature is usually adequate to produce full hardness, but oil quenching is sometimes used, particularly for larger sections. Parts should be tempered as soon as they have cooled to room temperature, particularly if oil quenching has been used, to avoid delayed cracking. Parts sometimes are frozen to approximately -75C before tempering to transform retained austenite, particularly where dimensional stability is important, such as in gauge blocks made of grade 440C. Tempering at temperatures above 510C should be followed by relatively rapid cooling to below 400C to avoid "475C" embrittlement. Some precipitation-hardening stainless steels require more complicated heat treatments than standard martensitic types. For instance, a semi-austenitic precipitation-hardening type may require annealing, trigger annealing (to condition austenite for transformation on cooling to room temperature), sub-zero cooling (to complete the transformation of austenite) and aging (to fully harden the alloy). On the other hand, martensitic precipitation-hardening types (such as Grade 630) often require nothing more than a simple aging treatment.

TEMPERING After hardening, most alloys are tempered to reduce brittleness and to relieve some of the high internal stresses developed during hardening. Tempering always follows, rather than precedes, the hardening process. Tempering is occasionally done after materials have been normalized, but its major use is after hardening. In some alloy steels tempering may increase hardness when tempered to certain temperature ranges. In most other materials, however, tempering causes an unavoidable loss of some hardness. The amount of hardness removed by tempering depends upon the tempering temperature; the higher the temperature, the softer the material will be. Tempering is always done at temperatures below the lower transformation point. In this respect, tempering differs from hardening, annealing, and normalizing, which all involve heating the material to temperatures above the upper transformation point. The temperatures used for tempering are selected on the basis of the properties required in the final product. For example, permanent magnets are tempered at 121F because they must retain considerable strength and hardness. Casehardened objects are also tempered at relatively low temperatures (212 to 400F) because the surface of such objects must remain hard. Many cutting tools are tempered at 430F or below so they will retain hardness. Battering tools must have great impact resistance and must be able to cut or penetrate metal; therefore, battering tools are tempered between 450 and 600F even though the higher temperatures mean some sacrifice of hardness to produce impact resistance. Springs are tempered between 600

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and 900F because the property of elasticity is more important in a spring than the property of hardness. Tools made of high-speed steels are tempered at 1,050 to 1,100F. Note, however, that with high-speed tools the high tempering temperature increases, rather than decreases, hardness. This increase in hardness occurs because high-speed steels retain austenite during quenching; when the hardened steel is tempered, the austenite changes to martensite. Since tempering uses temperatures below the lower transformation point, the rate of cooling generally has no effect upon the structure of the material. However, some nickel-chromium steels and a few other special steels become brittle if they are heated to the tempering temperature and then allowed to cool slowly. These steels, which are often called temper brittle or blue brittle steels, must be quenched rapidly from the tempering temperature to prevent brittleness. In general, however, steels are cooled SAMPLING
The choice of a sample for microscopic study may be very important. If a failure is to be investigated, the sample should be chosen as close as possible to the area of failure and should be compared with one taken from the normal section. If the material is soft, such as nonferrous metals or alloys and non-heat treated steels, the section may be obtained by manual hack sawing and if the material is hard, the section may be obtained by use of an abrasive cutoff wheel. This wheel is a thin disk of suitable cutting abrasive rotating at high speed. The specimen should be kept cool during the cutting operation

ROUGH GRINDING OR FILING.

Whenever possible, the specimen should be of a size that is convenient to handle. A soft sample may be made flat by slowly moving it up and back across the surface of a flat smooth file. The soft or hard specimen may be rough-ground on a belt sander, with the specimen kept cool by frequent dropping in water during the grinding operation In all grinding and polishing operations the specimen should be moved perpendicular Fig. Filing operation to the existing scratches This will facilitate recognition of the stage when the deeper scratches have been replaced by shallower ones characteristic of the finer abrasive, The rough grinding is continued until the surface is flat and free of nicks, burrs, etc. and all scratches due to the hacksaw or cutoff wheel are no longer visible.

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MOUNTING
Specimens that are small or awkwardly shaped should be mounted to facilitate intermediate and final polishing. Wires, small rods, sheet metal specimens, thin sections. etc., must be appropriately mounted in a suitable material or rigidly clamped in a mechanical mount. Synthetic plastic materials applied in a special mounting press will yield mounts of a uniform convenient size (usually 1 in, 1.25 in., or 1.5 in. in diameter) for handling in subsequent polishing operations. These mounts when properly made, are very resistant to attack by the etching reagents ordinarily used. The most common thermosetting resin for mounting is Bakelite, Bakelite molding powders are available in a variety of colors, which simplifies the identification .of mounted specimens The specimen and the correct amount of Bakelite powder, or a Bakelite perform, are placed in the cylinder of the mounting press. The temperature is gradually raised to 150oC, and a molding pressure of about 4,000 psi is applied simultaneously. Since Bakelite is set and cured when this temperature is reached, the specimen mount may be ejected from the molding die while it is still hot. Lucite is the most common thermoplastic resin for mounting. Lucite is completely transparent when properly molded. This transparency is useful when it is necessary to observe the exact section that is being polished or when it is desirable for any other reason to see the entire specimen in the mount. Unlike the thermosetting plastics, the thermoplastic resins do not undergo curing at the molding temperature; rather they set on cooling. The specimen and a proper amount of Lucite powder are placed in the mounting press and are subjected to the same temperature and pressure as for Bakelite (150oC 4,000 psi) after this temperature has been reached. The heating coil is removed, and cooling fins are placed around the cylinder to cool the mount below 75 oC in about 7 min while the molding pressure is maintained. Then the mount may be ejected from the mold. Ejecting the mount while still hot or allowing it to cool slowly in the molding cylinder to ordinary temperature before ejection will cause the mount to be opaque.

Small specimens may be conveniently mounted for metallographic preparation in a laboratory-made clamping device. Thin sheet specimens, when mounted in such as clamping device are usually alternated with metal "filler (sheets which have approximately the same hardness as the specimens. The use of filler sheets will preserve surface irregularities of the specimen and will prevent, to some extent, the edges of the specimen from becoming rounded during polishing.

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INTERMEDIATE POLISHING After mounting, the specimen is polished on a series of emery papers containing successively finer abrasives. The first paper is usually No. 3(36), 2.5(46), 2(60), 1.5(80), 1(100), 0(120). The intermediate polishing operations using emery paper are usually done dry; however, in certain cases such as the preparation of soft materials, silicon carbide abrasive may be used. As compared to emery paper, silicon carbide has a greater removal rate and. as it is resin-bonded, can be used with a lubricant. Using a lubricant prevents overheating the sample, minimizes smearing of soft metals, and also provides a rinsing action to flush away surface removal products so the paper will not become clogged. FINE POLISHING The time consumed and the successes of fine polishing depend largely upon the care that was exercised during the previous polishing steps. The final approximation to a fiat scratch-free surface is obtained by use of a wet rotating wheel covered with a special cloth that is charged with carefully sized abrasive particles. A wide range of abrasives is available for final polishing. While many will do a satisfactory job, there appears to be a preference for the gamma form of aluminum oxide for ferrous and copper-based materials, and cerium oxide for aluminum, magnesium, and their alloys. Other final polishing abrasives often used are diamond paste, chromium oxide, and magnesium oxide. The choice of a proper polishing cloth depends upon the particular material being polished and the purpose of the metallographic study. Many cloths are available of varying nap or pile, from those having no pile, such as silk, to those of intermediate pile, such as broadcloth, billiard Cloth, and canvas duck, and finally to a deep pile, such as velvet. Synthetic polishing cloths are also available for general polishing purposes, of which two, under the trade names of Gamal and Microcloth, are most widely used. A properly polished sample will show only the nonmetallic inclusions and will be scratch free.

Fig. Scratch-free surface after final polishing. Magnification 5OX. Black spots are oxide impurities.

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ETCHING The purpose of etching is to make visible the many structural characteristics of the metal or alloy. The process must be such that the various parts of the microstructure may be clearly differentiated. This is accomplished by use of an appropriate reagent which subjects the polished surface to chemical action. In alloys composed of two or more phases, the components are revealed during etching by a preferential attack of one or more of these constituents by the reagent, because of difference in chemical composition of the phases. In uniform single-phase alloys or pure metals, contrast is obtained and grain boundaries are made visible because of differences in the rate at which various grains are attacked by the reagent .This difference in the rate of attack is mainly associate with the angle of the different grain sections to the plane of the polished surface Because of chemical attack by the etching reagent, the grain boundaries will appear as valleys in the polished surface. Light from the microscope hitting the side of these valleys will be reflected out of the microscope, making the grain boundaries appear as dark lines.

TABLE Etching Reagents for Microscopic Examination

ETCHING REAGENT COMPOSITION

Nitric acid (nital) Picric acid (picral)

Ammonium per sulfate Palmerton reagent

Ammonium molybdate

Hydrofluoric acid

White nitric acid Ethyl or methyl alcohol (95% or absolute) (also amyl alcohol) Picric acid Ethyl or methyl alcohol (95% or absolute) Ferric chloride Hydrochloric acid Water Ammonium hydroxide Water Hydrogen peroxide Ammonium persulfate Water Chromic oxide Sodium sulfate Water Molybdic acid (85%) Ammonium hydroxide (sp gr 0.9) Water Filter and add to nitric acid (sp gr 1.32) Hydrofluoric acid (conc.) H2 O

1-5 ml 100 ml 4g 100 ml 5g 50 ml 100 ml 5 parts S:parts 2-5 parts 10 g 90 ml 200 g 15 g .1,000 ml 100 g 140 ml 240 ml 60 ml 0.5 ml 99.5 ml

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Fig. Photograph obtained from electron microscope after annealing.

WORKPIECE SPECIFICATION
Material: Mild Steel Type: Round Shaped Diameter: 25 mm Height: 10 cm Furnace temperature: 703o C

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DISCUSSION
From this experiment we are taught to learn the process of examining the microstructure of mild steel after heat treatment. The process was time consuming and a lot of care was necessary. The heating was done with care and accuracy. Filing was necessary to be done in only one way to avoid unwanted scratches. Nital was quite dangerous and it had to handle very carefully.

CONCLUSION
Success in microscopic study depends largely upon the care taken in the preparation of the specimen. The most expensive microscope will not reveal the structure of a specimen that has been poorly prepared. The procedure to be followed in the preparation of a specimen is comparatively simple and involves a technique which is developed only after constant practice. The ultimate objective is to produce a flat, scratch-free, mirror like surface.

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