MARMARA UNIVERSITY ENGINEERING FACULTY DEPARTMENT OF METALLURGICAL & MATERIALS ENGINEERING MSE-206 Materials Laboratory Experiment #6 : Annealing, Normalizing,Quenching

and Tempering of Steel Prepared By Ali Haydar ZCAN Student No 520070003 Submitted To Prof. Dr. A.Nihat GLLOLU Asst. smail TOPU Date of Experiment 27.04.2010 04.05.2010 Date of Report 18.05.2010

1. INTRODUCTION
This is a report including two experiment. The purpose of the experiments are to study the effect of the cooling rate and the amount of alloying elements on the microstructure and the mechanical properties (Rockwell hardness) of medium carbon steels ; effects of quenching and tempering of plain carbon eutectoid steel on its microstructure and its mechanical properties. The experiments can be expanded to investigate the effects of the carbon content on the mechanical properties and micro-structure of plain carbon steel.(1)

2. BACKGROUND
Iron-carbon phase diagram Iron-carbon phase diagram describes the iron-carbon system of alloys containing up to 6.67% of carbon, discloses the phases compositions and their transformations occurring with the alloys during their cooling or heating. Carbon content 6.67% corresponds to the fixed composition of the iron carbide Fe3C. The diagram is presented in the Figure.1 below. The following phases are involved in the transformation, occurring with ironcarbon alloys: L - Liquid solution of carbon in iron; -ferrite Solid solution of carbon in iron. Maximum concentration of carbon in -ferrite is 0.09% at 2719 F (1493C) temperature of theperitectic transformation. The crystal structure of -ferrite is BCC (cubic body centered). Austenite interstitial solid solution of carbon in -iron. Austenite has FCC (cubic face centered) crystal structure, permitting high solubility of carbon up to 2.06% at 2097 F (1147 C). Austenite does not exist below 1333 F (723C) and maximum carbon concentration at this temperature is 0.83%. -ferrite solid solution of carbon in -iron. -ferrite has BCC crystal structure and low solubility of carbon up to 0.25% at 1333 F (723C). -ferrite exists at room temperature. Cementite iron carbide, intermetallic compound, having fixed composition Fe3C. Cementite is a hard and brittle substance, influencing on the properties of steels and cast irons. The following phase transformations occur with iron-carbon alloys: Alloys, containing up to 0.51% of carbon, start solidification with formation of crystals of -ferrite.Carbon content in -ferrite increases up to 0.09% in course solidification, and at 2719 F (1493C) remaining liquid phase and -ferrite perform peritectic transformation, resulting in formation of austenite. Alloys, containing carbon more than 0.51%, but less than 2.06%, form primary austenite crystals in the beginning of solidification and when the temperature reaches the curve ACM primary cementite stars to form.

Iron-carbon alloys, containing up to 2.06% of carbon, are called steels. Alloys, containing from 2.06 to 6.67% of carbon, experience eutectic transformation at 2097 F (1147 C). The eutectic concentration of carbon is 4.3%. In practice only hypoeutectic alloys are used. These alloys (carbon content from 2.06% to 4.3%) are called cast irons. When temperature of an alloy from this range reaches 2097 F (1147 C), it contains primary austenite crystals and some amount of the liquid phase. The latter decomposes by eutectic mechanism to a fine mixture of austenite and cementite, called ledeburite. All iron-carbon alloys (steels and cast irons) experience eutectoid transformation at 1333 F (723C). The eutectoid concentration of carbon is 0.83%. When the temperature of an alloy reaches 1333 F (733C), austenite transforms to pearlite (fine ferrite-cementite structure, forming as a result of decomposition of austenite at slow cooling conditions).

Figure.1 Iron Carbon Phase Diagram(2) Isothermal Transformation Curves Since phase diagrams do not tell us anything about the kinetics of phase transformations another type of diagram is needed to determine whether or not equilibrium microstructures will be produced during cooling these diagrams are called isothermal transformation diagrams (ITD), or time-temperature-transformation (TTT) curves. The axes on a TTT plot are temperature versus log time. Isothermal transformation diagrams are constructed from a series of Avrami curves Consider the transformation of austenite to pearlite in a eutectoid steel: There are several key features of the partial TTT plot (i.e. pearlite) shown in Figure.2 i. Austenite maintained above the eutectoid temperature is stable, whereas the austenite region below the eutectoid temperature (and to the left of the pearlite start line) is considered unstable

ii. The curves are determined by very quickly reducing the temperature from the region of stable austenite to a lower value and then holding the new temperature constant until the transformation has completed. iii. A distinction can be made between coarse pearlite and fine pearlite (ie. thick vs. thin lamellae) based on the location at which a given cooling scheme passes through the pearlite region on the TTT diagram. If the pearlite curve in Figure.2 is continued to include all possible austenite decompositions, the complete TTT curve for eutectoid steel is produced. The complete curve contains several points of interest: austenite can transform into any combination of 3 possible phases the characteristic shape of the pearlite nose and bainite bay are indicative of the contradictory dependency of driving force on temperature versus mobility on temperature for most phase transformations produced upon cooling III. the martensite start and finish lines are purely horizontal, indicating that these transformations are athermal (ie. no thermal activation required) IV. any transformed austenite will not re-transform if the temperature is changed I. II.

Figure.2 TTT curve showing austenite to pearlite tranformation(5)

Quenching: Quenching is in many ways the most critical step in the process of heat-treating operations. The aim of quenching is to preserve the solid solution produced at the solution heat-treating temperature, by rapidly cooling to a lower temperature, usually near room temperature.

In most cases, the solid solution formed during solution heat treatment must be quenched rapidly enough to produce supersaturated solution at room temperature - the optimum condition for precipitation hardening. Annealing: Annealing is a heat process in which a metal is heated to a specific temperature and then allowed to cool slowly. This softens the metal which means it can be cut and shaped more easily. Mild steel, is heated to a red heat and allowed to cool slowly. However, metals such as aluminium will melt if heated for too long. 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. Normalizing: Normalizing is the process of raising the temperature to over 60 C (108 F), fully into the Austenite range. It is held at this temperature to fully convert the structure into Austenite, and then removed form the furnace and cooled at room temperature. 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 experiment conditions of cooling. This process is considerably cheaper than annealing since there is no need for a controlled furnace cooling. The main difference between annealing and normalizing is that fully annealed parts are uniform in softness throughout the entire part; since the entire part is exposed to the controlled furnace cooling. In the case of the normalized part, the cooling is non-uniform resulting in non-uniform material properties across the part. Tempering: Tempering is a heat treatment technique for metals, alloys and glass. In steels, tempering is done to toughen the metal by transforming brittle martensite into a combination of ferrite and cementite. Precipitation hardening alloys, like many grades of aluminum and superalloys, are tempered to precipitate intermetallic particles which strengthen the metal. Tempering is accomplished by a controlled reheating of the work piece to a temperature below its lower critical temperature. The brittle martensite becomes tough and ductile after it is tempered. Carbon atoms were held in the austenite when it was rapidly cooled, forming the martensite. The martensite becomes strong after being tempered because when reheated, the microstructure can rearrange and the carbon atoms can diffuse out of the distorted body-centred-tetragonal (BCT) structure. After the carbon diffuses, the result is nearly pure ferrite with body-centred structure. Hardness: Since the aging strengtens the material as mentioned above. The strenght of an aged material can be measured by hardness tests. Hardness is an extensive practice to test most materials before being confirmed for processing, and before being put into emamination to decide whether or not they meet the specifications needed. One of these tests is for hardness.

Hardness is a characteristic of a solid material expressing its resistance to permanent or plastic deformation. There are three general types of hardness measurements: (1) scratch hardness, (2) Indentation hardness, and (3) rebound or dynamic hardness. Among three only indentation hardness is of major engineering interest for metals. Some of the scales used for indentation hardness in engineering - Rockwell, Vickers, Brinell, and Knoop - can be compared using practical conversion tables for a particular material. The different techniques are shown in Figure-1. The most important ones of these testes are Brinell and Rockwell hardness tests. Rockwell Hardness Test The penetrators for the Rockwell hardness tester range from 1/2-inch diameter steel balls to very smalldiamond (brale) tips (points). The smaller points are used for harder materials that have a greater resistanceto indentation. There are various force scales used for various materials. The Rockwell B scale issuitable for soft engineering metals, and the Rockwell C scale is appropriate for hard engineering metals. Each scale requires a specified tip and load. The B scale uses a 1/16- inch diameter hardsteel ball and a 100-kg load. The C scale uses a conical diamond point and a 150-kg load. To perform the Rockwell tests, the penetrator is pressed against the specimen with an initial 10-kg preload to properly seat the penetrator. The remaining load is applied gradually after the dial on the hardness tester has been zeroed. After the penetrator has stopped moving into the specimen, the final position of the dial pointer indicates the Rockwell hardness number that is related to the depth of penetration.

Figure-3. Rockwell Harness Test

3. PROCEDURE
- Equipments:

Figure-4. Nabertherm Furnace (30 3000 C)

Table-1. Specification of Hardness Tester(4) Test Loads (kgf) Max Test Height Load Application Depth of Throat Magn. of Microscope 60, 100, 150 (Rockwell) 62.5, 187.5 (Brinell) With sliding table 140mm Hydraulic 145 mm 75x Brinell, 150x Vickers

Figure-5. Bulut Hardness Tester(4)

Furnace Hardness testers Gloves Tong Vessel 1080 steel 4140 steel 1040 steel Construction steel Lama steel Exp 1 1. Cut two small pieces 12 mm x 12 mm from the plain carbon steel stock, and two similar pieces from the low alloy steel stock. 2. Remove burrs from the samples by filing or grinding and stamp an identification code on each sample.

3. Place each sample in a small resistance furnace which is set at the proper austenitizing temperature, about 845C. The temperature of the furnace will first drop then recover again to the set temperature. Keep each specimen in the furnace half an hour after the 4. temperature returns to its initial setting. 5. Take one plain carbon steel specimen and one low alloy steel specimen out of the furnaces and let them cool down to room temperature (place them on a refractory tile or a brick in still air). As explained in your textbook, this is called a normalizing operation. 6. Furnace cool the other two specimens (one plain carbon steel and one low alloy steel). This is achieved by shutting off the furnace while keeping its door closed and the specimen inside, thus ensuring a very low cooling rate, which can actually be determined. This operation is called annealing. Remember, this takes a very long time so you can let the furnace cool down overnight. 7. Measure the Rockwell hardness of each specimen. If possible, use scale B or even scale A, so that the Rockwell hardness of the two annealed and two normalized specimens would fall on the same scale, thus facilitating comparison. 8. Prepare a micro section from each specimen for metallographic examination, and take a photomicrograph for each specimen. 9. Compare the Rockwell hardness of the different specimens as well as their photomicrographs and try to draw a correlation between the microstructure and the Rockwell hardness. Exp 2 1. Cut six specimens 12 mm x 12 mm from the stock and removes burr by filing and/or grinding. 2. Stamp the specimens for identification and determine the average Rockwell hardness for each. Be careful not to take hardness measurements near any stamped area. 3. Set aside one of the specimens for later metallographic examination, and put each of the others in a furnace with the temperature set at 830C, about l00C above AC3 as indicated by the phase diagram. The temperature of the furnace will drop slightly; as soon as it recovers, start measuring 45 minutes. 4. After the austenitizing time elapses, take each specimen out of the furnace quickly and drop it in an appropriate quenching tank containing two to four liters of water (about one-half to one gallon of water for each specimen). 5. Take the specimens out of the water and measure the Rockwell hardness of each. 6. Set aside one specimen for later metallographic examination and place the other into of 205C, 315C, 425C and 540C respectively. This process is called tempering. 7. After tempering the specimens for 45 minutes, take them out and allow them to cool down. 8. Measure the Rockwell hardness for each of these tempered specimens and plot a graph indicating hardness versus tempering temperature. Using horizontal lines of different colors, also show the original hardness of the as-received specimen as well as the hardness after quenching.

4. RESULTS
After completing the procedure steps, we can easily get average values of hardness and construct the Tables.( see appendix). Using these tables the following graph might be sketched.

Figure-6 Hardness vs. Temperature graph

5. DISCUSSION OF RESULTS
Normalizing and annealing processes that carried out at experiment 1 shows us low carbon steels (construction steel, lama) are relatively softer than medium carbon steels. The comparison between normalizing and annealing processes leads us that normalized specimens are tougher than the annealed specimens which is relevant to cooling rate. The quenching and annealing process that carried out at experiment 2 shows us that martensite is harder and brittle than tempered martensite. Also we can see that as the tempering temperature increases, hardness value of the specimen is decreases.

6. CONCLUTION
At first experiment, we examined the effects of annealing and normalizing processes on the mechanical properties of plain carbon steels and low alloy steels, leading us to AISI 4140 steel has the maximum hardness value, lama has the minimum hardness value. At second experiment, we examined tempering and quenching processes for the effects of the mechanical properties of plain carbon eutectoid steel, leading us to quenched specimen

has the maximum hardness value and the increase in temperature, decreases the hardness and increases the ductility.

7. RECOMMENDATION
Heat treatment processes should carried with high care because of the high temperatures. Tong and gloves must be use for safety. In annealing process specimens must be given more time to cool. In quenching process specimens must be dropped to quenching tank from furnace very quickly to prevent slow cooling.

8. BIBLIOGRAPHY
1. Prof. Dr. GLLOLU, Nihat and Research Assist. TOPU, smail, MSE 206 Materials Laboratory Lecture Reprints and Laboratory Manual , Winter 2006 2. http://www.davistownmuseum.org/PDFs/Pub42_Glossary_Appendix1_Iron%20Carbon%20Diagr
ams.pdf

3. Materials Science And Engineering An Introduction, William D. Callister, Jr.- 7. Edition 4. http://www.keytometals.com/Article39.htmhttp://www.bulutmak.com/enshowItems.php?ca t=29 5. http://www.sv.vt.edu/classes/MSE2094_NoteBook/96ClassProj/examples/kimttt.html

9. APPENDIX
Table-2. Experiment-1 datas ( 845 C) Steel 1040 1080 4140 Construction Lama Annealing (HRF) 74 81 80 58 53 Normalizing (HRF) 81 90 89 67 64

Table-3. Experiment-2 datas HRF 1. 2. 3. 4. 5. Average 845 C Martensite 68 65 69 70 71 68,6 205 C Tempered 62 63 62 63 64 62,8 315 C Tempered 57 58 58 61 59 58,6 425 C Tempered 49 48 48 47 48 48 540C Tempered 42 44 42 43 42 42,6