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Institute for Materials Applications in Mechanical Engineering (IWM), RWTH Aachen University, Augustinerbach 4, 52062 Aachen, Germany
_
Metal Forming Center of Excellence (MFGE), Atlm University, Kzlcasar Mah., 06836 Incek-Glbas
, Ankara, Turkey
a r t i c l e
i n f o
Article history:
Received 6 September 2015
Received in revised form 10 November 2015
Accepted 14 November 2015
Available online 2 December 2015
Keywords:
Tempering
Multiscale modeling
Precipitation simulation
Microstructureproperty relationships
AISI H13
a b s t r a c t
In the first part of this two part study, the mechanical properties necessary for the simulation of tempering of an AISI H13 (DIN 1.2344, X40CrMoV5-1) tool steel was derived using physically based precipitation
simulations and microstructureproperty relationships. For this purpose, the precipitation of fine
carbides were simulated using a thermo-kinetic software which allows prediction of the evolution of precipitation/dissolution reactions and the particle sizes. Then, those microstructural findings were coupled
with physically based microstructureproperty models to predict the yield stress, flow curve and creep
properties. The predicted mechanical properties were verified with corresponding experiments and a
good agreement was found. In the second part of this study, those properties were coupled with a
Finite Element (FE) model in order to predict the relaxation of internal stresses and the evolution of deformations at the macroscopic scale.
2015 Elsevier B.V. All rights reserved.
1. Introduction
Hot-work tool steel AISI H13 (DIN 1.2344, X40CrMoV5-1) is
mainly used as tools for extrusion, forging dies and especially as
die-casting dies for the processing of light metals. AISI H13 has distinguished mechanical properties like high hardness, good wear
resistance, thermo-cyclic stability and high strength at elevated
temperatures which are essential for high temperature tool applications. These properties can be generated only by a controlled
heat treatment process which consists of an austenitization treatment with a subsequent hardening and a multiple tempering procedure. The superior mechanical properties are due to the
nanometer size alloy carbides which precipitate during the tempering. In order to predict the mechanical properties of AISI H13
during and after tempering, the development of those carbides
should be well known. The chemical composition of the investigated steel is given in Table 1.
There are several attempts in the literature which concentrate
on predicting the macroscopic material properties from the
microstructural parameters. Most of the previous work in the liter-
Corresponding author.
E-mail address: caner.simsir@atilim.edu.tr (C. Simsir).
http://dx.doi.org/10.1016/j.commatsci.2015.11.020
0927-0256/ 2015 Elsevier B.V. All rights reserved.
281
Table 1
Chemical composition of steel AISI H13 (wt%).
C
Cr
Ni
Mo
Mn
Si
0.40
5.37
1.34
1.22
0.3
0.97
2. Modeling
rfe 78 0:023 T
rss
f
X
n
K iXi i
i1
rP
Ncoh
Ntotal
1=2 q
1=2
N
r2chem r2coh r2mod incoh
ro
Ntotal
where Ncoh ; N incoh ; N total are the number densities of the coherent,
the incoherent and the sum of the number densities of precipitates,
respectively. The terms in the second square root are the strength
contributions due to chemical hardening effect (rchem ), the coherency strain effect (Misfit strengthening) (rcoh and the modulus
hardening effect (rmod ). The final term (ro ) in Eq. (4) is the strength
contribution of the impenetrable precipitates.
The chemical hardening term (rchem ) is described by the general
FriedelBrownHam equation [26]:
rchem
2M
bkC1=2
cb
3=2
1=2
N
r2
b
where r represents the mean precipitate radius, G is the shear modulus, e is the linear misfit strain, and N is the corresponding number
density.
The modulus strengthening effect is due to the intersection of
dislocations with a spherical precipitate having a shear modulus
lower than the shear modulus of the matrix. The formulation based
on the work of Russell et al. [27]:
282
Table 2
Parameters K and n from Eq. (3) (for carbon from [3,24,4,25] and other alloying elements from [23]).
K i (MPa/wt%)
ni ()
rmod M
Al
Cr
Mn
Mo
Nb
Ni
Si
1171:3
1=3
4000
0:75
1400
0:75
7000
0:75
9600
0:75
4000
0:75
6100
0:75
11000
0:75
4000
0:75
11000
0:75
"
2 #3=4
Gb
Up
1
k
Um
where U p and U m are the line energies of the dislocation in the precipitate (U p ) and in the iron matrix (U m ), respectively.
Finally the strengthening effect of impenetrable particles (ro ) is
described by the Orowan Mechanism [28]:
ro CM
Gb
ro
ln
k
ri
rdis a G b qdis
10
rsgb
115
2w
14
dw
Q
C w wexp m
dt
RT
15
where C w is a constant with a value of 1.4 103. After double tempering at 650 C for two hours the martensite lath width was calculated to be around 0.17 lm from Eq. 15.
G 0:039431 T 98:46456
11
where G is in GPa.
Bhadeshia et al. [3] proposed a general equation to determine
qdis of martensite at room temperature (RT) after quenching
depending on the martensite start temperature (M s in Kelvin)
logqdis 9:2840
6880:73 1780360
Ms
M 2s
12
dqdis
Q
C dis qdis exp v
dt
RT
13
dqdis M e_ pl
dt
bL
16
where e_ pl is the plastic strain rate, M is the Taylor factor. The mean
free path L is limited by the average spacing between dislocations:
A
L p
17
qdis
dqdis
dann
q Me_ pl
B2
dt
b dis
18
in which B is a constant depending on the different number of activated slip systems. The critical distance dann is described by [45]:
4
dann
Gb
2p1 mQ mf
19
283
m is the
dqd
Gb
C2Dd
q2 q2deq
dt
kB T dis
3
20
Dd ad Db
21
Especially for tool steels which are normally tempered for long
soaking times at elevated temperatures above 0:4T m , where T m is
the melting temperature of the steel, creep plays a major role on
the amount of stress relaxation.
The physically based creep model used in this work is based on
the composite model of Mughrabi et al. [48,49]. Blum et al. implemented this model to predict the high temperature creep behavior
of the martensitic steels [6,7,50,51]. The basic idea of the model is
that the heterogeneous dislocation distribution causes a heterogeneous stress distribution. Correspondingly the material is treated
as a composite of a hard (subscript h) phase with high dislocation
density and a soft (subscript s) phase with low dislocation density. It is assumed that the total strain etot is identical in both
regions:
rs
E
es
rh
E
eh
22
where etot is the sum of elastic and the plastic strain, E is the elastic
modulus, rs and rh are the local stress acting in soft and hard
region. The elastic strain is calculated by the terms rs =E; rh =E for
the soft and hard region respectively. es and eh are representing
the plastic strains in the corresponding regions. Due to the heterogeneous distribution of the dislocations, internal forward stresses
rf are formed at the (hard) subgrain boundaries corresponding to
internal back stresses rb in the subgrain interior. The local stresses
rs and rh can be defined as:
rs rA rb ;
23
rh rA rf ;
24
where
r
etot 1 f h es f h eh
rA f s rs f h rh :
25
26
where the first term rE is the elastic strain and the plastic strain
epl is defined by Eq. (27) as follows:
epl 1 f h es f h eh :
27
Differentiating Eq. (27) for the case of creep (r = constant) gives the
plastic deformation rate:
e_ pl 1 f h e_ s f h e_ h f_ h eh es
28
where e_ s and e_ h are the deformation rates in the soft and hard
region of subgrains respectively. The local deformation rates are
formulated as:
e_ s
b
q ms ;
M dis
29
e_ h
b
q mh ;
M dis
30
with ms and mh the velocity of the dislocations in soft and hard region
and defined by Eqs. (31) and (32) respectively.
mh v h;0 sinh
2.5. Creep
etot
In Eq. (25), the terms f h and f s is the volume fraction of the hard
and soft regions. The volume fraction of hard region is defined as
f h a 2=w (a = width of hard region, 2=w: subgrain boundary area
per volume) and for the soft region as f s 1 f h , so that the total
strain can be calculated from Eqs. (22) and (25) as:
31
!
32
Q
B As exp s
RT
v h;0 Ah exp
33
Q
h
RT
34
35
rh rh rp;h :
36
The effective stress in a soft region r is described as the difference between the local stress in soft regions rs and the stress components resulting from the interaction with other free dislocations
rdis and precipitates rp;s . On the other side, the effective stress in
hard regions rh is defined as the difference between the local stress
in the hard region rh and the stress component resulting from the
interaction with other free precipitates rp;h . The athermal stress
component rdis which results from the interaction of the free dislocations, is calculated using Eq. (9). The stress component rp;s
resulting from particle hardening in soft regions can be formulated
with particle size dp and the average volume fraction f p of the
precipitates.
s
37
284
rOrowan:s 3:32 G b
q
Np
f p;s;k
X
k1
38
dp;k
where N p is the number of precipitates. The phenomenological relationship between the parameter C p;s and the local stress rs is
described by Eq. (35).
rs
1 exp
C1
C p;s
C 2 !!1=C2
39
f p;s;k
1 Up;SGB
f p;k
1 f p;SGB
40
p dp;k 3
f p;SGB 1 1 p
2 6 w
41
rp;h
2
f p;h;k
Eo X
b 1 dp;k
42
f p;h;k f p;k
Up;SGB
43
f p;SGB
The evolution of the microstructure during creep can be formulated from the equations above. The parameters of the dislocation
structure are the mean subgrain size w, the spacing between free
dislocations in the subgrain interior q0:5
, the width of the hard
f
region a, and the spacing s between the dislocations in the subgrain
boundaries. Their steady state values (after creep) designated by
the subscript 1 are given by the equations:
w1 10
bG
jrj
q0:5
dis;1 3:9
bG
jrj
s1 1:5 b
a1
44
45
0:5
46
jrj
0:05 w1
2
47
log f log f1 logfo =f1 exp
e
kf
48
Under constant loading (creep), the rate of the local stress in the
soft region can be calculated by differentiation of Eq. (23):
r_ s f h Ee_ h e_ s f_ h
rs r
fh
49
Eq. (49) was integrated over the plastic strain, so that the development of the plastic strain rate during creep can be achieved. The
necessary material and microstructure parameters for the modeling
of creep is summed up in Table 3.
3. Results and discussion
3.1. Precipitation
For realistic simulation of the precipitation evolution during
annealing, the initial precipitation state should be known. In this
work, the initial microstructure (carbide size, carbide content)
after austenitization and quenching was determined from the
scanning electron microscope (SEM) investigations [52]. The
undissolved carbides after austenitization and quenching found
to be MC carbides with a volume fraction of 0.65 vol% and average
radius of 57.01 nm. In order to define the initial state, a so called
Virtual Pre Treatment in MatCalc was conducted. The parameters
of the Virtual Pre-Treatment can be arbitrarily selected so that
the phase fraction and the size of the carbides in the initial structure are consistent with the experimentally determined values.
After several iterative Virtual Pre Treatment simulations, the calculated carbide phase fraction and the average radius of the MC
carbides matched with the experimental findings, which describes
the initial state before tempering.
The carbide types and the possible nucleation sites considered
in the simulation were selected to be the same as in the previous
work of Sonderegger [53] where a similar hot-work tool steel
was investigated (Table 4). Furthermore dislocation density and
subgrain size were given as input for the simulation of precipitation during tempering, whose values were discussed already in
the previous section.
The simulation of the precipitation development during tempering was conducted for three different tempering temperatures;
520, 600 and 650 C (Figs. 13). 520 C is the tempering temperature, where the maximum hardness can be achieved [56]. 600 C
is a common tempering temperature for this kind of steels and
650 C is towards the highest temperature, that the hot-work tool
steel can be tempered. The heating and cooling times were selected
as 0.5 h and the soaking time at the corresponding tempering temperature as 2 h. The diagrams show only the secondary hardening
carbides, which precipitate during tempering. Phase fraction and
size of MC carbides, which do not dissolve during austenitization,
change only slightly during tempering.
For all of the tempering temperatures, cementite was formed
during the heating to the tempering temperature in the first tempering step and dissolves rapidly at the tempering temperature.
The M7C3 carbides were formed rapidly upon reaching the tempering temperature and the phase fraction was higher than all the
other carbides except for the tempering temperature of 650. However, its fraction decreases with further soaking time. In contrast,
the fraction of the second Cr rich carbide namely M23C6 increases
gradually during the tempering. For the tempering temperature
of 650 C, M23C6 carbide has the highest volume fraction in comparison with the other carbides. The calculated phase fraction of
M6C carbide has its maximum value during tempering at 600 C.
The phase content of this carbide also rises gradually with the
increasing tempering time, except during tempering at 650 C, like
the M23C6 carbide. However, the calculated phase portion of this
carbide was lower than that of the other carbides except for the
285
Value
Source
kw
ka
kqdis;0
[38]
[2]
[7]
[7]
[7]
[7]
[7]
ks
C 1 rOrowan;s
C 2 rOrowan;s
Eq. (48)
Eq. (39)
Eq. (39)
0.0005
116:37 53:54 ln0:25 rOrowan;s 21:65
[7]
[7]
[7]
Eq. (10)
[1]
b
G
Qs
Qh
As
Ah
Bs
b
n
Burgers vector
Shear modulus
Activation energy (soft region) Eq. (33)
Activation energy (hard region) Eq. (34)
Eq. (33)
Eq. (34)
Eq. (31)
Eq. (31)
Eq. (31)
0.248 (nm)
Eq. (11)
562 (kJ/mol)
562 (kJ/mol)
3.59 1015 (m/s Pa)
4.39 1020 (m/s)
9.0 1019 (m/Pa s)
0.59
0.045
[7]
[6]
[7]
[7]
[7]
[7]
[7]
w0
qdis;0
s0
Up;SGB
Table 4
Carbide types and their possible nucleation sites which were considered in the
precipitation simulations.
Carbide type
MC
M23C6
M7C3
M6C
Cementite (M3C)
Grain boundary,
Grain boundary,
Grain boundary,
Grain boundary,
Dislocations
Subgrain
Subgrain
Subgrain
Subgrain
boundary, Dislocations
boundary
boundary
boundary
carbides (Fig. 3). Although the M7C3 carbide shows coarsening with
increasing tempering temperatures, the coarsening rate, when
compared with the M23C6 carbide was very low. However, the
coarsening of the M7C3 carbide is faster than the MC and M6C carbides. The M6C carbide has a higher resistance to coarsening, especially at elevated temperatures. The size of the carbide was higher
at the tempering temperatures of 520 C and 600 C than that of
MC carbide, however, the size of the carbide after tempering at
650 C was almost equal to be the size of the MC carbide. Finally,
the mean radius of the MC carbide after each tempering temperature was calculated as the smallest compared to the other carbides.
Fig. 4 shows the results of the calculated phase fraction and the
carbide size of the secondary hardening carbides after two times
tempering at the corresponding tempering temperatures. The total
fraction of the secondary carbides corresponds to about 5.6 vol.% at
520 C, 5.8 vol.% at 600 C and 5.3 vol.% at 650 C. In the work of
Ebner et al. [54] the phase fraction of secondary carbides was
determined for the steel X38CrMoV5-3 as 4.5 vol.% for the austenitization temperature of 1050 C. Although the exact tempering
temperature was not mentioned in the work, the tempering
Fig. 1. Kinetic simulation of the precipitate evolution of steel AISI H13 during tempering at 520 C: (a) tempering temperaturetime profile; (b) phase fraction; (c) mean
precipitate radius; and (d) number density.
286
Fig. 2. Kinetic simulation of the precipitate evolution of steel AISI H13 during tempering at 600 C: (a) tempering temperaturetime profile; (b) phase fraction; (c) mean
precipitate radius; and (d) number density.
Fig. 3. Kinetic simulation of the precipitate evolution of steel AISI H13 during tempering at 650 C: (a) tempering temperaturetime profile; (b) phase fraction; (c) mean
precipitate radius; and (d) number density.
Fig. 4. Simulated phase fraction and mean radius after two times tempering at the tempering temperatures of 520 C, 600 C, and 650 C.
287
288
Fig. 5. Simulated precipitation strengthening rp during tempering compared with the experimental findings: (a) Tempering temperature 520 C. (b) Tempering
temperature 600 C. (c) Tempering temperature 650 C.
Fig. 6. Simulated yield stresses and the corresponding strengthening terms during tempering compared with the experimental findings: (a) Tempering temperature 520 C.
(b) Tempering temperature 600 C. (c) Tempering temperature 650 C.
curve is known aside the yield strength. For this reason, simulations of the flow curves during tempering are required. The critical
point during tempering where the stress relaxation (time independent) due to the drop of yield stress can occur should be where the
tempering temperature is just reached. After reaching the tempering temperature, the time dependent relaxation due to creep
289
Fig. 7. Simulated flow curves at the corresponding tempering temperatures (immediately after reaching the tempering temperature) compared with the experimental
findings: (a) Tempering temperature 520 C. (b) Tempering temperature 600 C. (c) Tempering temperature 650 C.
each other. At this point it should be once more pointed out, that
especially for the first tempering due to the higher instability of
the microstructure at elevated temperatures, the measured values
has higher uncertainty [52]. Considering this, a better agreement of
the measured and calculated flow curves for the second tempering
cycle can be observed from Fig. 7 as expected.
3.4. Creep
Especially for steels with higher tempering temperatures, creep
(time-dependent/viscous deformation) is the major stress relaxation mechanism during tempering. The experimental observation
showed that short term creep effect for the steel AISI H13 becomes
significant for the tempering temperatures of 600 C and 650 C
[52]. In contrary to the instant compression tests conducted during
the tempering to determine yield stress and the corresponding
flow curves, the creep experiments were conducted on three times
tempered specimen, so that a stable microstructure before the
experiments is assured. During tempering, the microstructure is
instable. The compression tests to determine flow curves were relatively short, the effect of microstructure evolution during the test
can be neglected. However during a short term creep test (10 h) of
a not tempered martensite, the tempering process takes place during the test itself which will affect the measurements remarkably.
Consequently creep experiments were simulated only for the tempering temperatures of 600 C and 650 C for three times tempered
martensite under the loads of 400, 500 and 600 MPa.
The mathematical model of creep was programmed in Matlab
and solves the differential equation (Eq. (49)) with the Matlab
Solver ode45. In Table 1, the required microstructure and material parameters for the simulation of creep are summarized. In
addition to those parameters, the model requires for the description of the Orowan stress (rOrowan:s , Eq. (38)) the volume fraction
and the size of the carbides. These two parameters were calculated
by MatCalc and the creep model is taking those parameters from
the precipitation simulations. Two other parameters b and n (Eq.
(31)) used for the description of the dislocation velocity in the soft
region (Subgrain interior) were required to be estimated as in the
reference work [7]. In this work, these parameters were determined in Matlab by the optimization function fmincon. The
calculated parameters b and n are given in Table 1.
The simulation results and their comparison with the experimentally determined strain rate during loading is shown in
Fig. 8. Although the overall shape of the calculated curves particularly for smaller strains up to 0.004 at the tempering temperature
of 600 C, deviates from the experimental curves, the model predicts the minimum creep rate e_ min very well. It should be noted
that the initial microstructure for the creep tests at 600 C and
650 C are completely different, while the specimens were tempered for three times at the corresponding tempering temperatures. This effect was taken into account in the model with the
consideration of the dislocation density, subgrain size, volume
fraction and size of carbides.
One of the simplest material models to describe creep in the
macroscopic scale is Nortons creep law, where the stress dependency of the steady state creep rate e_ c is described in a power
law:
e_ c Ac rnc
50
Fig. 8. Simulated creep curves at the corresponding tempering temperatures compared with the experimental findings: (a) Tempering temperature 600 C. (b) Tempering
temperature 650 C.
290
Table 5
Parameter Ac and nc for the power law at temperatures 600 C and 650C.
Ac (s1 MPanc )
600 C
650 C
nc ()
Exp.
Sim.
Exp.
Sim.
6.72393 1013
1.59987 1023
3.47308 1013
2.80594 1022
2.06132
6.57970
2.17178
6.12114
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