M2 Effects of Tempering Temperatures on Hardened High Alloy Steel Objective To determine the effects of hardening and tempering on high

alloy steel, and to compare the mechanical properties (hardness, impact energy and ductility) of hardened high alloy steel different tempering temperatures. Materials and Equipment: Furnace Rockwell hardness tester, Charpy impact tester, six standard specimens of high alloy steel K110 for Charpy impact test, Metallurgical microscope, 2% Nital acid. Introduction and Background Information: Hardening is heating and then cooling at such a rate of steel alloys so that a significant increase in hardness occurs. In most cases, hardening is performed in connection with a subsequent new heating, the tempering. If, after hardening at a high temperature, tempering is performed and then a relatively low hardness combined with high toughness is achieved, this process is called hardening and tempering. The hardening process of workpieces can be divided into three technical steps. First, the workpiece is heated so that the output structure transforms into an austenitic structure. This austenitizing temperature depends on the material used (750 C 1210 C). Then the workpiece is maintained at this temperature so that alloying elements can be incorporated homogenously in this austenitic structure. The final step is quenching the workpiece at such a cooling rate that a so-called martensitic structure is originated. Steel has in an unhardened state a body centered cubic (BCC) structure, in which it can only dissolve very little carbon. After warming up over approx. 720 C austenite is originated that has a body face centered (BFC) crystal structure (and occupies a smaller volume). It can dissolve considerably more carbon, which occurs at hardening temperature. By cooling the material then rapidly enough, converting it from a cubic face centered crystal structure back into a cubic spatially centered structure, oversatured carbon remain and martensite is originated. Due to the presence of supersaturated carbon, the BCC (body centered cubic) lattice is stretched out to a

tetragonal lattice. The martensite thus possesses high internal stresses and a larger volume than non-hardened steel at room temperature. As a consequence, the high internal stresses have a high hardness of the material. Upon tempering, a little carbon will be diffused from the tetragonal cube. Consequently stress and volume, but also hardness decrease and the toughness increases significantly.

Figure 1: Crystal structure in hardening process

Tempering should be carried out within a reasonable time after hardening, preferably within an hour or so. It is of vital importance that the steel should be allowed to cool to room temperature before tempering is started. The transformation to martensite will otherwise be interrupted and the hardening results may be impaired. A higher tempering temperature will yield a somewhat softer material with higher toughness, whereas a lower tempering temperature will produce a harder and somewhat more brittle material, as shown by the figure below.

Figure 2: Effects of tempering temperature on the hardness and toughness

Procedure: 1. The test specimen is marked from 1 to 6 by using a punch at the end of the specimen and the furnace temperature is set to 1040oC.

2. The Rockwell hardness reading of each of the specimens is measured using the C scale. (Reading is taken voiding the region close to the notch)

3. The specimens form number 2 to 6 is put into the furnace when the temperature reached 1040 oC. The specimens are quenched in the water solution. The specimens are dried and the scales are removed with sand papers. The Rockwell hardness values of each of the specimens are measured. 4. Specimen number 3 is placed into furnace at 200 oC 30 minutes and the it is colled down in air. Specimens 4,5 and 6 are placed into the furnace at 325 oC, 450 oC and 650 oC respectively for 30 minutes.

5. When tempering process is done, the Rockwell hardness test is performed for every specimen and followed Charpy impact test. The readings are recorded and tabulated.

6. Metallographic examinations on every specimens is done and the microstructure are captured.

Results:
Specimen Process 1 none 2 hardening 3 hardening + tempering 200C 4 hardening + tempering 325C 5 hardening + tempering 450C 6 hardening + tempering 650C

Hardness Test Specimen HRC 1 HRC 2 HRC 3 HRC average 1 (as received) 20.2 18.9 23.8 20.96666667 2 63.7 63.8 64.3 3 59.9 59.8 59.6 4 60.2 60 59.5 59.9 5 69.9 65.5 64.7 6 58.1 56.8 59.2

63.93333333 59.766667

66.7 58.03333

Table 1: Hardness (as received and after hardening)

Specimen (tempering temp, C) HRC 1 HRC 2 HRC 3 HRC average 3(200) 57.1 57.5 57.2 57.26666667 4(325) 55.2 54.6 55.5 5(450) 51.5 52.2 50 6(650) 42 39.6 42.4

55.1 51.233333 41.33333

Table 2: Hardness (after tempering) *Note: 1. We do not perform any hardening and tempering on specimen 1 2. For specimen 2, we only conduct hardening on it, no tempering

Charpy Test
Specimen Thickness at v-notch (S, cm) Thickness (D, cm) Width (B, cm) Cross-Sectional Area at v-notch (SxB cm2) 1 0.821 1.006 1.064 2 0.917 1.029 1.101 3 0.886 1.061 1.006 4 0.964 1.174 0.998 5 0.873 1.034 1.013 6 0.919 1.014 1.083

0.874

1.010

0.891

0.962

0.884

0.995

Table 3: Dimension of Charpy impact specimen

Lifting up Specimen angle (, ) 1 136.5 2 136.5 3 136.5 4 136.5 5 136.5 6 136.5 Table 4: Angle before and after swing

Angle at the end of swing (, ) 130 132.5 131.5 133 133 134.5

Specimen (Processes)

1 (As received) 2 (Hardening only) 3 (Hardening and tempering at 200C ) 4 (Hardening and tempering at 15.10 325C) 5 (Hardening and tempering at 15.10 450C) 6 (Hardening and tempering at 8.52 650C) Table 5: Toughness value of Charpy impact test

E (Absorbed Energy Before Fracture, J) 28.76 17.34 21.85

K (Toughness Value, J/cm2) 32.91 17.17 24.52 15.70 17.08 8.56

Fracture surface:

Specimen 1: As-received

Specimen 2: Hardened

Specimen 3: 200oC Tempered

Specimen 4: 325oC Tempered

Specimen 5: 450oC Tempered

Specimen 6: 600oC Tempered

Microstructure:

Specimen 1: As-received

Specimen 2: Hardened

Specimen 3: 200oC Tempered

Specimen 4: 325oC Tempered

Specimen 5: 450oC Tempered

Specimen 6: 600oC Tempered

Note: 1000x Magnification

Calculations:

E (Amount of absorbed energy, J) = MgD ( cos cos ) A (Cross-sectional area of specimen at v-notch) = b x s W (Mass of hammer) = 41.76kg R (Length of Hammer) = 0.85m g (Gravitational force) = 9.81 m/s (Lifting up angle) = 136.5 (Angle at the end of the swing) = As show in table above for each specimens

Specimen 1 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 130 cos 136.5) = 28.76 J

K = E/A = 28.76 / 0.874 = 32.91 J/cm2

Specimen 2 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 132.5 cos 136.5) = 17.34J K = E/A = 17.34 / 1.01 =17.17 J/cm2

Specimen 3 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 131.5 cos 136.5) = 21.85 J K = E/A = 21.85 / 0.891 =24.52 J/cm2

Specimen 4 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 133 cos 136.5) = 15.10 J K = E/A = 15.10 / 0.962 =15.70 J/cm2 Specimen 5 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 133 cos 136.5) = 15.10 J K = E/A = 15.10 / 0.884 =17.08 cm2

Specimen 6 E = WgR( cos cos ) = (41.76) (9.81) (0.85) (cos 134.5 cos 136.5) = 8.52 J K = E/A = 8.52 / 0.995 =8.56 cm2

Discussion: a) Hardness as a function of tempering temperature for specimens 3, 4, 5 and 6.

Hardness value,HRC against tempering temperature,C

70 60 Hardness Value, HRC 50 40 30 20 10 0 2(hardening) 3(200) 4(325) 5(450) 6(650) Specimen (tempering temp, C) 63.933 57.267 55.100 51.233 41.333

Figure 3: Graph of hardness value, HRC against different tempering temperature of specimens 2, 3, 4, 5 and 6. From the graph plotted above, the relationship between the tempering temperature, C and the hardness value, HRC has been observed. The highest HRC value obtained in this experiment is sample 2 which undergoes only hardening process. The hardness value of specimen 3, 4, 5 and 6 are 57.27,55,1, 51,23 and 41.33 respectively. For specimen that undergoes tempering process, specimen 3 has the highest HRC value whereas specimen 6 has the lowest HRC value. It is observed that the HRC value decreases when the tempering temperature is increases. The hardness of K110 high alloy steel is continuously decreasing with increasing of tempering temperature. It can be said that the hardness of the steel is inversely proportional to the tempering temperatures.

b) Toughness as a function of tempering temperature for specimens 2, 3, 4, 5 and 6.

Toughness Value, J/cm2 against tempering temperature, C

30 25 Toughness Value, J/cm2 20 17.170 15 10 5 0 2 (Hardening only) 3 (200C ) 4 (325C) 5 (450C) 6 (650C) Specimen (tempering temp, C) 15.700 17.080 24.520

8.560

Figure 4: Graph of toughness value, J/m2 against different tempering temperature of specimens 2, 3, 4, 5 and 6. From the graph plotted above, the relation between the tempering temperature, C and the toughness value, K has been observed. The specimen which having the highest toughness value is sample 3 which is 24.52J/cm2 while the specimen with the lowest toughness value is specimen 6 which is 8.56 J/ cm2. Specimen 2 which does not going through any tempering shows a toughness value of 17.17 J/ cm2. Toughness value of specimen 2 is lower specimen 3 where tempering process has been done. Theoretically, with increasing tempering temperature, the toughness value will be increased. However, the toughness value of specimen 4 and 5 are lower than specimen 3 while the toughness value for specimen 6 is the lowest. These phenomenon will be discussed in the following.

Information from microstructure, Hardness Value and Toughness Value. In specimen 1, the microstructure is observed that it contained pearlite, ferrite and carbide structure. Specimen 2 shows fine needle like martensite structure with retained austenite and residual carbides. The martensite structure is formed due to quenching which increased the cooling rate. The structure is highly stressed with high hardness but very brittle. Specimen 3 has been tempered at 200 C. The microstructure show tempered martensite which the fine needle like structure is reduced. There is a small quantity of retained austenite and residual carbides. The hardness decreases compared to specimen 2 but the toughness increases significantly. As the tempering temperature goes higher, in specimen 4, 5 and 6, it is observed that the fine martensitic structure become lesser because it has been into tempered martensite. In specimen 4, the retained austenite changes into ferrite and carbides structure. The hardness decreases, but the toughness also decreases. This may due to temper embrittlement. Temper embrittlement is caused by the presence of specific impurities in the steel, which segregate to prior austenite grain boundaries during heat treatment. The main embrittling elements (in order of importance) are antimony, phosphorous, tin and arsenic. In specimen 5, the martensite structure has been changed into tempered martensite structure. The retained autenite has been fully transformed into ferrite and carbide structure. The hardness decreases and the toughness increases. For specimen 6, the martensite is transformed back to ferrite and carbide structure hence carbide formation become coarser. The hardness continue decreasing but the toughness value shows in practical is the lowest. Theoretically, sample 6 supposed to show the highest toughness value because it is tempered with high temperature of 650 C. However, the experimental results show lowest value in its toughness. This might due to the effect of secondary hardening, which the carbide will reprecipitate at the grain boundary and caused the structure to lose its ductility. But, the fracture surface observed on specimen 6 shows rough fracture surface. Rough surfaces mean the specimen is ductile. Which mean the specimen undergo some plastic deformation before failure occurs. Ductile structures will have low hardness, but high toughness value. The low toughness value of specimen 6 obtained may be due to other experimental error such as human error. There might be some mistake that has been done while taking the readings in the experiment such as the dimensioning of the specimen or recording the angle of the end of swing while doing impact test.

Tempering Tempering is an important process to be done subsequent to quench hardening. Quenchhardened parts are often too brittle. This brittleness is caused by the forming of martensite and also internal stresses formed when quenched. This brittleness can be removed by tempering. Tempering results in a desired combination of hardness, ductility, toughness, strength, and structural stability. Tempering consists of heating the steel to a specific temperature (below its hardening temperature), holding it at that temperature for the required length of time, and then cooling it, usually instill air. This will release the internal stresses. The resultant strength, hardness, and ductility depend on the temperature to which the steel is heated during the tempering process. The mechanism of tempering depends on the steel and the tempering temperature. The prevalent martensite is a somewhat unstable structure. When heated, the carbon atoms diffuse from martensite to form a carbide precipitate and the concurrent formation of ferrite and cementite, which is the stable form. Tempering on Hardened Alloy Steel The general effect of the alloying elements in alloy steel is to retard the softening rate, so these alloy steels will require a higher tempering temperature to obtain a given hardness than carbon steel of the same carbon content. However, the individual elements show significant differences in the magnitude of their retarding effect. Nickel, silicon, aluminum and, to a large extent, manganese, which have little or no tendency to occur in the carbide phase, and merely remain dissolved in ferrite, have only a minor effect on the hardness of the tempered steel - an effect that would be expected from the general pattern of solid-solution hardening. Chromium, molybdenum and vanadium, on the other hand, which migrate to the carbide phase when diffusion is possible, bring about a retardation of softening, particularly at the higher tempering temperatures. These elements do not merely raise the tempering temperature. When they are present in higher percentages, the rate of softening is no longer a continuous function of the tempering temperature. That is, the softening curves for these steels will show a range of tempering temperature in which the softening is retarded or, with relatively high alloy content, in

which the hardness may actually increase with increasing tempering temperature. This characteristic behavior of the alloy steels containing the carbide-forming elements is known as "secondary hardening" and results presumably from a delayed precipitation of fine alloy carbides. Secondary Hardening Secondary hardening is the transformation of retained austenite to martensite causing an increase in hardness. This frequently occurs in high alloy tool and high speed steels due to precipitation of carbides during the tempering process. High alloy grades of tool steel may require three or four tempering cycles for complete transformation. A number of the familiar alloying elements in steels form carbides, which are thermodynamically more stable than cementite. Nitrogen and boron are increasingly used in steels in small but significant concentrations. The alloying elements Cr, Mo, V, W and Ti all form carbides with substantially higher enthalpies of formation, while the elements nickel, cobalt and copper do not form carbide phases. Manganese is weak carbide former, found in solid solution in cementite and not in a separate carbide phase. It would, therefore, be expected that when strong carbide forming elements are present in steel in sufficient concentration, their carbides would be formed in preference to cementite. Nevertheless, during the tempering of all alloy steels, alloy carbides do not form until the temperature range 500-600C, because below this the metallic alloying elements cannot diffuse sufficiently rapidly to allow alloy carbides to nucleate. The metallic elements diffuse substitutionally, in contrast to carbon and nitrogen which move through the iron lattice interstitially, with the result that the diffusivities of carbon and nitrogen are several orders of magnitude greater in iron, than those of the metallic alloying elements. Consequently, higher temperatures are needed for the necessary diffusion of the alloying elements prior to the nucleation and growth of the alloy carbides and, in practice, for most of the carbide forming elements this is in the range 500-600C. This secondary hardening process is a type of age-hardening reaction, in which relatively coarse cementite dispersion is replaced by new and much finer alloy carbide dispersion. On attaining a critical dispersion parameter, the strength of the steel reaches a maximum, and as the carbide dispersion slowly coarsens, the strength drops.

Conclusions: The effects of hardening and tempering on high alloy steel have been determined. The HRC value is of the highest for specimen that only go through hardening process. The hardness of hardened high alloy steel is continuously decreasing with increasing of tempering temperature. It can be said that the hardness of the steel is inversely proportional to the tempering temperatures. In contrast, with increasing tempering temperature, the toughness value will be increased. In conclusion, the impact energy and ductility increases with the increase of tempering temperature.

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http://www.simplytoolsteel.com/heat-treating-tempering-tool-steel.html [Accessed: 8 Jul 2013]. 5. T. V. Rajan & C. P. Sharma & Ashok K. Sharma. Heat Treatment: Principles and Techniques, 1992. New Delhi: Prentice-Hall of India Private Ltd.