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900 Temperature, C 800 700 600 500 400 300 0 15 30 45 60 75 Time, min 90 105 120 135

Furnace temp. + Load max. exper. Load min. exper. Load max. calcul. Load min. calcul.

FIGURE 6.111 Computer simulation for heating of shafts. (From M.A. Aronov, J.F. Wallace, and M.A. Ordillas, System for prediction of heat-up and soak times for bulk heat treatment processes, Proceedings of the International Heat Treatment Conference on Equipment and Processes, April, 1820, 1994, Schaumburg, IL, pp. 5561.)

require different graphs. The correction factor k depends on the type of steel. The generalized equation (Equation 6.43) for the heat-up and soak time determination was set into a userfriendly computer package that incorporates charts for the calculation. This resulted in a straightforward way of determining the soak time without the use of charts while allowing for a quick and accurate soak time calculation.

6.3.2 QUENCHING INTENSITY MEASUREMENT

AND

EVALUATION BASED ON HEAT FLUX DENSITY

In designing the method for practical measurement, recording, and evaluation of the quenching and cooling intensity in workshop conditions, in contrast to the Grossmann H value c ic was concept, which expresses quenching intensity by a single number, the main idea of Lis to express the quenching intensity by continuous change of relevant thermodynamic functions during the whole quenching process. Instead of recording only one cooling curve (as in laboratory-designed tests) in the center of a small (usually 1/2 in.) cylindrical specimen, the

300 250 N=4

N=3

N=2 N = Number of trays

Soak time (tsb), min

200 150 N>4 100 50 0 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7 N=1

Load characteristic size, in.

FIGURE 6.112 Thermal soak time for a packed load. (From M.A. Aronov, J.F. Wallace, and M.A. Ordillas, System for prediction of heat-up and soak times for bulk heat treatment processes, Proceedings of the International Heat Treatment Conference on Equipment and Processes, April, 1820, 1994, Schaumburg, IL, pp. 5561.)

2006 by Taylor & Francis Group, LLC.

heat flux density at the surface of a standard-size probe becomes the main feature in measuring, recording, and evaluating the quenching intensity. The first substantial difference between using the small laboratory specimen and using the probe applied in the method described below is that when quenching, for example, in an oil quenching bath, because of its small mass and small heat capacity the former will cool down in 1530 s, whereas the latter will take 500600 s to cool to the bath temperature, allowing the entire quenching process of real components to be followed. This workshop-designed method is applicable to 1. All kinds of quenchants (water and brine, oils, polymer solutions, salt baths, fluid beds, circulated gases) 2. A variety of quenching conditions (different bath temperatures, different agitation rates, different fluid pressures) 3. All quenching techniques (direct immersion quenching, interrupted quenching, martempering, austempering, spray quenching) The method is sufficiently sensitive to reflect changes in each of the important quenching parameters (specific character of the quenchant, its temperature, and mode and degree of agitation). This method
.

Enables a real comparison of the quenching intensity among different quenchants, different quenching conditions, and different quenching techniques Provides an unambiguous conclusion as to which of two quenchants will give a greater depth of hardening (in the case of the same workpiece and same steel grade) and enables the exact calculation of cooling curves for an arbitrary point on a round bar cross section of a specified diameter, to predict the resulting microstructure and hardness (an exception is the case of delayed quenching, where the cooling rate is discontinuously changed; for an explanation see Ref. [23]) Furnishes information about thermal stresses and possible superposition of structural transformation stresses that will occur during a quenching process Provides the basis for automatic control of the quenching intensity during the quenching process

The method itself, known in the literature as the temperature gradient method, is based on the known physical rule that the heat flux at the surface of a body is directly proportional to the temperature gradient at the surface multiplied by the thermal conductivity of the body material: ql dT dx (6:44)

where q is the heat flux density (W/m2) (i.e., quantity of heat transferred through a surface unit perpendicular to the surface per unit time); l is thermal conductivity of the body material (W/(m K)), and dT/dx is the temperature gradient at the probe surface perpendicular to the surface (K/m). The essential feature of the method is a cylindrical probe [32] of 50-mm diameter 200 mm, instrumented with three thermocouples placed along the same radius at the halflength cross section as shown in Figure 6.113. As can be seen, the thermocouple at the surface reproducibly measures the real surface temperature of the probe (Tn), which is important to register all the phenomena that are taking place on the surface during quenching. The intermediate thermocouple (Ti) measures the temperature at a point 1.5 mm below the surface. The readings of Tn and Ti enable the heat treater to easily calculate the temperature gradient near the surface of the probe at each moment of cooling. The central thermocouple

2006 by Taylor & Francis Group, LLC.

Tc

Tn

Ti 1.5 N5

Diam. 50

All dimensions in mm

c ic -NANMAC probe (made by the NANMAC Corp., Framingham Center, FIGURE 6.113 The Lis MA) for measurement of the temperature gradient on the surface.

(Tc), placed at the center of the cross section, indicates how long it takes to extract heat from the core and provides at every moment the temperature difference between the surface and the core, which is essential for the calculation of thermal stresses. Specific features of probe are the following: 1. The response time of the surface thermocouple is 105 s; the fastest transient temperature changes can be recorded. 2. The intermediate thermocouple can be positioned with an accuracy of +0.025 mm. 3. The surface condition of the probe can be maintained by polishing the sensing tip before each measurement (self-renewable thermocouple). 4. The body of the probe, made of an austenitic stainless steel, does not change in structure during the heating and quenching process, nor does it evolve or absorb heat because of structural transformation. 5. The size of the probe and its mass ensure sufficient heat capacity and symmetrical radial heat flow in the cross-sectional plane where the thermocouples are located. 6. The heat transfer coefficient during the boiling stage, which, according to Kobasko [22], depends on bar diameter, becomes independent of diameter for diameters greater than 50 mm.

2006 by Taylor & Francis Group, LLC.

100

200

When a test of the quenching intensity is performed, the probe is heated to 8508C (15628F) in a suitable furnace and transferred quickly to the quenching bath and immersed. The probe is connected to the temperature acquisition unit and a PC. Adequate software enables the storage of the temperaturetime data for all three thermocouples and the calculation and graphical display of relevant functions. The software package consists of three modules: Module I. TEMP-GRAD (temperature gradient method) Module II. HEAT-TRANSF (calculation of heat transfer coefficient and cooling curves) Module III. CCT-DIAGR (prediction of microstructure and hardness after quenching) As an example let us compare two different quenching cases: Case A. Quenching in a mineral oil bath at 208C (688F) without agitation (Figure 6.114a through Figure 6.114f) Case B. Quenching in a 25% polyalkalene glycol (PAG) polymer solution at 408C (1048F) and 0.8 m/s agitation rate (Figure 6.115a through Figure 6.115f) By comparing Figure 6.114b and Figure 6.115b it is clear that case B involves delayed quenching with a discontinuous change in cooling rate, because in case A the time when maximum heat flux density occurs (tqmax) is 15 s whereas in case B it is 72 s. In case A (oil quenching), by 20 s after immersion (see Figure 6.114e) the extracted amount of heat was already 34 MJ/m2, and by 50 s, it was 50 MJ/m2, whereas in case B (high concentration polymer solution quenching; see Figure 6.115e) by 20 s, the extracted heat was only 5 MJ/m2 and by 50 s this value was only 20 MJ/m2. However, immediately after that in the period between 50 and 100 s, in case A the extracted amount of heat increased from 2 2 50 to only 55 MJ/m , whereas in case B it increased from 20 to 86 MJ/m . Both of the calculated integral ( q dt) curves, designated with the open square symbols in Figure 6.114e and Figure 6.115e, have been calculated as the area below the heat flux density vs. time curves, designated similarly in Figure 6.114b and Figure 6.115b. That is, they represent the heat extracted only through the surface region between the point 1.5 mm below the surface and the surface itself. Comparing the time required to decrease the heat flux density from its maximum to a low value of, e.g., 100 kW/m2 (see Figure 6.114b and Figure 6.115b), one can see that in case A 45 s is necessary, whereas in case B only 28 s is necessary. This analysis certifies that case B (quenching in PAG polymer solution of high concentration) is a quenching process with delayed burst of the thick polymer film. Discontinuous change in cooling rate is inherent to this quenching regime. In this respect it is interesting to analyze the cooling rate vs. surface temperature diagrams of Figure 6.114f and Figure 6.115f. While in oil quenching (case A), the cooling rate at the surface of the probe (*) has a higher maximum than the cooling rates at 1.5 mm below the surface (&) and at the center (D), in case B the maximum cooling rate at 1.5 mm below surface (during a certain short period between 350 and 3008C (662 and 5728F) surface temperature) is higher than the maximum cooling rate at the surface itself. This can also be seen in Figure 6.115a, which shows that the slope of the cooling curve Ti between 500 and 3008C (932 and 8428F) is greater than the slope of the cooling curve for the very surface (Tn). This is another experimental proof that in delayed quenching cooling rates below the workpiece surface can be higher than at the surface itself. Another analysis, with respect to thermal stresses during quenching (on which the residual stresses and possible distortion depend), is possible by comparing Figure 6.114d and Figure 6.115d. This comparison shows that quenching in a PAG polymer solution of high

2006 by Taylor & Francis Group, LLC.

concentration (case B), compared to oil quenching (case A), resulted in 27% lower maximum temperature difference (read thermal stress) between the center and surface of the probe (*) or 36% lower maximum temperature difference between the center and the point 1.5 mm below the surface, (D), contributing to lower distortion than in oil quenching. Whereas with oil quenching the maximum temperature difference between the center and the point 1.5 mm below the surface (D) is higher than the maximum temperature difference between the point

1000 900 800 Temperature T, C 700 600 500 400 300 200 100 0 1
1n 2i

Tc Ti Tn Measured 50 100 200 500 1000 Time t, s 50 100 200 500 1000 Time t, s Calculated
2i-n

2
3c

10

20

(a)
3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400 200 0
1c-n

Tn = surface temperature, T i = temperature 1.5 mm below the surface, Tc = temperature in the center of the probe.

Heat flux density q, kW/m2

1
2i-n

2
3c-i

10

(b)

20 tmax

3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400 200 0 0
1c-n

Heat flux density q, kW/m2

(c)

100 200 300 400 500 600 700 800 900 10001100 1200 Temperature Tn,C
3c-i

c ic FIGURE 6.114 Graphical display from Module I, TEMP-GRAD, when quenching the Lis NANMAC probe in a 208C mineral oil bath without agitation. (a) Measured and recorded temperature vs. time, T f(t); (b) calculated heat flux density vs. time, q f(t); (c) calculated heat flux density vs. surface temperature, q f(Tn).

2006 by Taylor & Francis Group, LLC.

Calculated

500 450 T, C Temperature differences 400 350 Calculated 1 2 2i-n 5 3c-i 10 20 50 100 200 500 1000 Time t, s 2 2i-n 3c-i 5 10 20 50 100 200 500 1000 Time t, s 5 0 0 100 200 300 400 500 600 700 800 900 10001100 1200 Temperature Tn,C 2i 3c Calculated Calculated 300 250 200 150 100 50 0

(d)

1c-n 100 90 80 70 dt, (MJ/m2) 60 50 40 30 20 10 0 1

(e)

t0

1c-n 50 45 40 Cooling rate dT, K/s dt 35 30 25 20 15 10

(f)

1n

FIGURE 6.114 (Continued ) (d) Calculated temperature differences vs. time, DT f(t). (e) Calculated integral q dt heat extracted vs. time. (f) Calculated cooling rates vs. surface temperature dT/dt f(Tn).

1.5 mm below the surface and the surface itself. (&), In the case of delayed quenching (case B), the maximum temperature difference between the point 1.5 mm below the surface and the surface itself (& in Figure 6.115d) is slightly higher than the maximum temperature defference between the center and the point 1.5 mm below the surface (D), which is reached about 20 s later. This also shows an abrupt heat extraction when the polymer film bursts. On the other hand, Figure 6.114d shows that in oil quenching the maximum temperature difference between the center and surface (*) occurs 20 s after immersion, when the surface temperature is 4508C (8428F) (see Figure 6.114a), i.e., above the temperature of the Ms point. In

2006 by Taylor & Francis Group, LLC.

PAG polymer solution quenching (Figure 6.115d), the maximum temperature difference between the center and the surface (*) occurs much later, when the surface temperature has already fallen to 3608C (6808F) (see Figure 6.115a). In this respect, dealing with steels that have a high Ms temperature, water-based polymer solutions always run a higher risk of overlapping thermal stresses with those created due to austenite-to-martensite transformation.

1000 900 800 Temperature T, C 700 600 500 400 300 200 100 0 1 1n 2 5 10 20 50 100 200 300 1000 Time t, s 2i 3c Tn = surface temperature, Ti = temperature 1.5 mm below the surface, TC = temperature in the center of the probe. Tn Tc Ti

(a)

Heat flux density q, kW/m2

3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400 200 0 1

2 2i-n

5 3c-i

10

20

(b)

1c-n 3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000 800 600 400 200 0 0 1c-n

30 100 200 500 1000 Time t, s Tqmax

Heat flux density q, kW/m2

(c)

100 200 300 400 500 600 700 800 900 1000 1100 1200 Temperature Tn , C 2i-n 3c-i Tqmax

c ic -NANFIGURE 6.115 Graphical display from Module I, TEMP-GRAD, when quenching the Lis MAC probe in a PAG polymer solution of 25% concentration, 408C bath temperature, and 0.8 m/s agitation rate. (a) Measured and recorded temperature vs. time data, T f(t). (b) Calculated heat flux density vs. time, q f(t). (c) Calculated heat flux density vs. surface temperature, q f(Tn).

2006 by Taylor & Francis Group, LLC.

Calculated

Calculated

Measured

500

Temperature differences T, C

450 400 350 300 250 200 150 100 50 0 1 2 5 10 20 50 100 200 300 1000

(d)

1c-n 2i-n 3c-i


200 180 460

Time t, s

q dt, MJ/m2

140 120 100 80 60 40 20 0 1 2 5 10 20 50 100 200 300 1000

tx

(e)

t0

1c-n 2i-n 3c-i


25

Time t, s

20

dT Cooling rate dt , K/S

15

10

100 200 300 400 500 600 700 800 900 1000 1100 1200

(f)

1n

2i

3c

Temperature Tn, C

FIGURE 6.115 (Continued ) (d) Calculated temperature differences vs. time, DT f(t). (e) Calculated integral q dt heat extracted vs. time. (f) Calculated cooling rates vs. surface temperature, dT/dt f(Tn).

The probability of crack formation can be seen at a glance by comparing the surface temperature of the probe at the moment the maximum heat flux density occurs (Tqmax). As seen in Figure 6.114c, Tqmax is 5158C (9598F) for oil quenching (case A), while for waterbased polymer solution (case B), Tqmax is 3808C (7168F) (see Figure 6.115c). The lower the value of Tqmax, the higher is the risk of crack formation, especially with steel grades having high Ms temperature.

2006 by Taylor & Francis Group, LLC.

Calculated

Calculated

Calculated

When direct immersion quenching is involved with continuous cooling (not delayed quenching with discontinuous cooling), the depth of hardening, when comparing two quench ing processes, is determined as follows: The larger the values of qmax and q dt and the shorter the time tqmax,, the greater will be the depth of hardening. Module II of the software package, HEAT-TRANSF, makes it possible (based on the input of measured surface temperatures and calculated heat flux density on the very surface) to calculate (by a numerically solved method of control volumes) and graphically present 1. The heat transfer coefficient between the probes surface and the surrounding fluid vs. time, a f(t) (Figure 6.116a) 2. The heat transfer coefficient between the probes surface and the surrounding fluid vs. surface temperature, a f(Tn) (Figure 6.116b) Using the calculated values of a, the software program enables the calculation of cooling curves at any arbitrary point of the round bar cross section of different diameters, as shown in Figure 6.117a and Figure 6.117b. The Module III of the software package, CCT-DIAGR, is used to predict the resulting microstructure and hardness after quenching of round bar cross sections of different diameters. This module contains an open data file of CCT diagrams in which users can store up to 100 CCT diagrams of their own choice. The program enables the user to superimpose every calculated cooling curve on the CCT diagram of the steel in question. From the superimposed cooling curves shown on the computer screen, the user can read off the percentage of structural phases transformed and the hardness value at the selected point after hardening as shown by Figure 6.118.
1800 1600 1400 1200 1000 800 600 400 200 0 0.01 0.1 1 10 100 1000

Heat transfer coefficient a , W/m2K

(a)

Time, s

Heat transfer coefficient a , W/m2K

1800 1600 1400 1200 1000 800 600 400 200 100 200 300 400 500 600 700 800 900

(b) 0 0

Temperature, C

FIGURE 6.116 Heat transfer coefficient (a) vs. time and (b) vs. surface temperature when quenching the c ic -NANMAC probe (50-mm diameter 200 mm) in a 208C mineral oil bath without agitation. Lis

2006 by Taylor & Francis Group, LLC.

900 800 700 Temperature, 8C 600 500 400 300 200 100 0 0.01 0.1 1 10 Time, s 100 1000

(a)

900 800 700 Temperature, C 600 500 400 300 200 100 0 0.01 0.1 1 10 Time, s 100 1000

(b)

FIGURE 6.117 Comparison of measured (- - -) and calculated () cooling curves for the center of a 50-mm diameter bar quenched in (a) mineral oil at 208C, without agitation and (b) 25% PAG polymer solution, 408C bath temperature, and 0.8 m/s agitation rate.
Chemical composition 1000 AISI 4140 900 800 3/4 R C 30 P 5 10 200 B 400 300 M 200 100 58 0 1 10 53 52 102 34 28 27 230 103 104 220 105 106 Ms 2 3 75 85 75 70 40 60 40 60 Ac3 Ac1 Austenitizing temp. 850 C C 0.38 Si 0.23 Mn 0.64 P S Cr Cu 0.17 Mo 0.16 Ni V

0.019 0.013 0.99

0.08 <0.01

Temperature, C

700 S 600 A 500 2 F 7

12

Time, s

FIGURE 6.118 CCT diagram of AISI 4140 steel with superimposed calculated cooling curves for surface (S), three-quarter radius (3/4R) and center (C) of a round bar of 50-mm diameter.

2006 by Taylor & Francis Group, LLC.

If for a round bar cross section of the chosen diameter the cooling curves are calculated at three or five characteristic points (surface, (3/4)R, (1/2)R, (1/4)R, center), using the HEATTRANSF module, the CCT-DIAGR module enables the user to read off the hardness values after quenching at those points and to obtain the hardness distribution curve displayed graphically on the computer screen. In the case of delayed quenching with discontinuous change of cooling rate, the prediction of structural transformations and hardness values after quenching from an ordinary CCT diagram is not correct because the incubation time consumed (at any point of the cross section) before the cooling rate abruptly changes has not been taken into account. For a detailed explanation see Shimizu and Tamura [11].

6.3.3 RETAINED AUSTENITE

AND

CRYOGENIC TREATMENT

The martensite start (Ms) and martensite finish (Mf) temperatures for unalloyed steels depend on their carbon content, as shown in Figure 6.119. As can be seen from this diagram, when steels of more than 0.65% C are quenched the austenite-to-martensite transformation does not end at room temperature (208C (688F)) but at some lower temperature, even at temperatures much lower than 08C (328F). Consequently, after these steels are quenched to room temperature, a portion of austenite will remain untransformed; this is referred to as retained austenite. The greater the amount of carbon in the steel, the greater the amount of retained austenite after quenching, as shown in Figure 6.120c. Retained austenite, which is a softer constituent of the structure, decreases the steels hardness after quenching. If present in amounts of more than 10%, a substantial decrease in the hardness of the quenched steel may result (see curve a of Figure 6.120a). When quenching hypereutectoid steels from the usual hardening temperature (Figure 6.120b) i.e., from the g Fe3C region, the same hardness will result independently of carbon content (curve b in Figure 6.120a), because the hardness of martensite depends only on the carbon dissolved in austenite (g), which further depends (according to the solubility limit, line SE) on the hardening temperature. The structure of hardened hypereutectoid steels therefore consists of martensite Fe3C retained austenite. When quenching hypereutectoid steels from the region of pure austenite (g), i.e., from above the Acm temperature (which is not usual), the structure after hardening consists only of martensite and retained austenite, and the hardness decreases with carbon content as shown

600 500 Temperature, 8C 400 300 200 100 20 0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 C, wt% Mf Ms

FIGURE 6.119 Martensite start (Ms) and martensite finish (Mf) temperatures vs. carbon content in unalloyed steels.

2006 by Taylor & Francis Group, LLC.

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