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Article history: Cryogenic treatments are considered a good way to reduce the retained austenite content and improve
Received 6 May 2014 the performance of tool steels. Four different heat treatments, two of which included a deep cryogenic
Received in revised form stage, were applied in this study to an H13 tool steel, subsequently determining its mechanical
2 October 2014
properties by means of tensile, hardness and fracture toughness tests. Furthermore, scanning electron
Accepted 17 November 2014
Available online 25 November 2014
microscopy and X-ray diffraction analysis were performed to gain an insight into the microstructural
evolution of these heat treatments during all the stages.
Keywords: It was concluded that the application of a deep cryogenic treatment to H13 steel induces higher
AISI H13 tool steel thermal stresses and structural defects, producing a dispersed network of ne carbides after the
Deep cryogenic treatments
subsequent tempering stages, which were responsible for a signicant improvement in the fracture
Mechanical properties
toughness of this steel without modifying other mechanical properties. Although the application of a
Microstructural evolution
X-ray diffraction deep cryogenic treatment reduces the retained austenite content, there is a minimum innate content
which cannot be transformed by heat treatment. Nevertheless, this austenite is hence believed to be
stable enough and should not transform during the normal service life of forging dies.
& 2014 Elsevier B.V. All rights reserved.
1. Introduction
As regards the service lifetime of dies, hot forging involves
Traditional hot forging manufacturers are constantly improving extreme working conditions which result in a series of life-limiting
productivity in order to be competitive and maintain or increase their failure mechanisms. Although dies are inevitably replaced after a
market share and prots. In this respect, there are three main reasons certain period of time, the aim is to maximize their lifetime. As die
why companies are investing to optimize their forging processes: the costs represent between 15 and 30% of the total costs for a closed
gradual increase in energy costs (electricity and gas) in recent years die forging process [3,4], producing more parts with the same die
[1], the competitiveness of rms from emerging countries, and the leads to a notable cost reduction. To do so, computer design and
development of more economic production technologies with good simulation software techniques are useful tools to improve the
mechanical properties, such as modern casting [2]. design of forging dies. Furthermore, material selection and heat
As a result, forging companies are forced to minimize their treatments (HT) are also factors of major importance [5].
production costs and achieve more efcient processes by means of Quenched and tempered H13 hot work tool steel is thus mainly
the following methods [3]: used to make hot forging dies in virtue of its excellent properties:
high hardness and mechanical strength, good toughness and
Reduction in labour costs via the increased use factory auto- signicant resistance to shock, thermal fatigue and wear [58].
mation systems. This paper discusses the performance of four different heat
Increasing the lifetime of forging dies. treatments applied to an H13 steel. Two different quenching media
Optimizing the use of available equipment. (gas and oil) and the effects of a cryogenic stage were studied.
Material optimization by reducing ashes and nishing In general terms, the application of deep cryogenic treatments
operations. to tool steels is acknowledged to provide the following benets: a
Shortening the design cycle. decrease in retained austenite content, a uniformly dispersed
network of ne carbides and a homogenized microstructure.
Reducing the retained austenite content is very convenient, as it
n
Corresponding author. Tel.: 34 985182024; fax: 34 985182022. enhances the dimensional stability of the dies, as reported by
E-mail address: marcosperezrd@gmail.com (M. Prez). Surberg et al. [9], leading to increased service lifetimes. The main
http://dx.doi.org/10.1016/j.msea.2014.11.051
0921-5093/& 2014 Elsevier B.V. All rights reserved.
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240 33
advantage of cryogenic treatments, on the other hand, seems to be parameters were carried out as per the UNE-EN ISO 6892-
that of modifying the carbide distribution pattern, as this mod- 1:2009 standard.
ication has a positive effect on hardness, mechanical strength, The hardness of the steel was determined by means of the
fracture toughness and structure homogeneity. The typical carbide Rockwell C hardness test using a HOYTOM hardness tester under a
morphologies present in tool steels are: quite large primary load of 150 kg. For treatments HT1 to HT4, samples were extracted
carbides, which do not dissolve during the austenitizing treat- from the non-deformed central section of the SENB specimens
ment, secondary microcarbides, which precipitate during quench- once the fracture toughness test was completed. Five indentations
ing, and secondary nanocarbides, which are formed during the were made in the thickness direction to appreciate any hardening
tempering stage [10,11]. It is worth noting that cryogenic treat- due to the cooling rate gradient existing between the surface and
ments only modify the nanocarbides precipitated during the the centre of the samples. Moreover, for samples 1 and 2, Rockwell
tempering stages, but primary and secondary carbides do not C hardness measurements were performed after each stage
experience any modication in their morphologies [11]. The (quenching (Q), deep cryogenic treatment (C) and tempering (T))
maintenance at 196 1C gives rise to a ne modulated structure of the overall heat treatment to appreciate the evolution of
with carbon enriched regions and structural defects. This structure hardness and to compare the results with the Full Width at Half
leads to a ner and more homogeneous carbide precipitation Maximum (FWHM) parameter, which was obtained in the course
during the tempering phase and to an increase in the volume of the X-ray diffraction analysis.
fraction of nanocarbides [10,12,13]. In line with bibliographic references [8,15], KIC fracture tough-
As a consequence of the transformation of the retained auste- ness tests following the ASTM E1820 standard [16] were carried
nite and the optimal carbide distribution, Baldissera et al. [14] out due to the fact that H13 steel is quite brittle at room
reported that cryogenic treatments produce a more homogeneous temperature. Three single edge notched bend (SENB) specimens,
structure which delays the nucleation of cracks and increases the each with a width (W) of 40 mm, a thickness (B) of 20 mm, a span
fatigue life of the tool. (S) of 160 mm (4 W) and a crack size-to-width ratio (a/W) of 0.45,
were tested for each heat treatment. Tests were performed on an
MTS tensile machine, equipped with a 100 kN load cell at a
2. Experimental methods displacement rate of 0.5 mm/min. Specimens had been fatigue
pre-cracked to the required nominal a/W using a load ratio of 0.1, a
2.1. Steel and heat treatments frequency of 3 Hz and a maximum stress intensity factor, K, of
25 MPa m1/2 in order to prevent sudden fracture of the speci-
An H13 steel regularly used to make hot forging dies was mens [15]. The conditional result, KQ, which was determined from
studied in this research. Its chemical composition is given in the load versus COD record according to the ASTM E1820 standard,
Table 1. was consistent with size and linear elastic requirements, so the
Tensile and fracture specimens were subjected to four different results obtained could be considered as material fracture tough-
heat treatments involving quenching and tempering. Two quench- ness (KIC) [16].
ing media (nitrogen gas and oil) and two types of sequences
(quenching (Q) tempering (T) and quenching (Q) cryogenic 2.3. Fractographic and microstructural characterization
treatment (C) tempering (T)) were carried out. The sequences
and characteristics of the applied treatments can be seen in Fractographic and microstructural analyses were carried out to
Table 2. understand and justify the mechanical testing results. The steel
Apart from the four sequences described above, an extended microstructures were studied by optical and scanning electron
study was conducted to gain an insight into the effects of deep microscopy. The latter technique was also used to characterise the
cryogenic treatments and assess the inuence of the other factors fracture surfaces.
of the studied heat treatments, such as quenching media and As far as microstructural examination is concerned, metallo-
tempering stages. Two 20 10 8 mm specimens (samples 1 graphic samples were prepared from the non-deformed central
and 2) were cut from the non-deformed central section of the section of the SENB specimens. These were ground, polished with
fracture specimens and were likewise subjected to the heat diamond paste and nally etched with picral. All samples were
treatments described in Table 2. In this case, the effect of quench rst observed under a Nikon Epiphot 200 optical microscope and
severity was studied, comparing oil and air as quenching media. then, under a FEG-SEM Carl Zeiss GEMINI microscope.
Fracture surfaces from the SENB specimens were likewise
2.2. Mechanical characterization analysed under a JEOL JSM-5600 scanning electron microscope
at different magnications to reveal the predominant failure
The mechanical properties of the H13 steel were measured at micromechanisms. This examination focused mainly on observing
room temperature by means of tensile, hardness and fracture tests. the onset zone of fracture growth from the fatigue pre-crack.
Tensile tests were performed on cylindrical tensile specimens
of 10 mm diameter with a calibrated length of 70 mm using a MTS 2.4. X-ray diffraction analysis
tensile machine equipped with a 250 kN load cell at a displace-
ment rate of 2 mm/min. Three specimens were tested for each X-ray diffraction was applied to determine the residual stress
heat treatment. In order to calculate elongation (e), an initial state induced in the heat treatments, the structural distortion, via the
gage length of 50 mm was considered on each specimen. The Full Width at Half Maximum (FWHM) parameter, and the retained
experimental procedure and the determination of the main austenite content. Measurements were performed for the four
applied heat treatments (HT1HT4), on the non-deformed central
Table 1 sections of the SENB specimens, as well as on samples 1 and 2.
H13 steel chemical composition (weight%). The FWHM parameter is considered an indicator of the struc-
tural distortion of the material. In particular, it is related to the
%C %Si %Mn %Cr %Mo %V dislocation density and to the existence of micro-residual stresses
0.39 1.0 0.4 5.2 1.4 0.9
[17]. As thermal and transformation stresses can give rise to local
plastic deformation and to an increase in dislocation density,
34 M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
two factors related to steel hardness, the FWHM parameter is the presence of carbides. In this case, therefore, the obtained
generally acknowledged as a complementary index to characterise results are only comparative.
the hardening of the steel [18,19].
In the present study, X-ray diffraction measurements were
performed on a Stresstech XSTRESS 3000 G3R diffractometer. In 3. Results
order to determine the residual stress state and the FWHM
parameter, the X-ray diffraction technique employed was the 3.1. Mechanical properties
sin2 method, following the recommendations by National Phy-
sical Laboratory (NPL) [20], while the determination of FWHM The tensile test (elastic modulus (E), yield strength (ys),
consisted in the analysis of the diffraction peak broadening. A Cr- ultimate tensile strength (UTS), elongation (e) and area reduction
K X-ray source was used, employing a wavelength of 0.2291 nm. (Z)) and hardness results are shown in Table 4. The differences
Measurements were taken on the (2 1 1) diffraction peak of the between the four heat treatments were not signicant, HT1 being
martensite, which was recorded at a 2 angle of approximately affording the highest yield strength and ultimate tensile strength.
1561, and the diffraction elastic constant of the selected diffraction Cryogenic treatments did not seem to affect the tensile properties
plane, E/(1 ), was 168,900 MPa [21]. Diffraction data were of the steel. No signicant differences in hardness were observed
determined in three different directions on the sample plane: between the different heat treatments either.
45, 0 and 451, subsequently calculating the average result. The In addition, the evolution of the average hardness throughout
longitudinal direction of the samples was designated as direction the overall heat treatment is shown in Fig. 1. It can be seen that the
01. Nine tilt angles () between -45 and 451, a 20-second highest hardness value was obtained after the quenching stage
exposure time for each single measurement and a 2 mm diameter due to the presence of a non-tempered hard martensite. As it will
collimator were also used. The diffraction peaks were processed be seen later, at the end of the cryogenic stage a certain amount of
via a Pseudo-Voigt adjustment and background noise was mini- retained austenite transforms into martensite, while a slight soft-
mized by means of a parabolic expression. ening of 0.7 and 0.6 HRC was observed for air and oil quenching,
The retained austenite content was calculated following the respectively. It seems that the early carbide precipitation during
experimental procedure explained in the ASTM E975-03 standard the heating stage from the cryogenic temperature ( 196 1C) to
and in [22]. Samples cut from the non-deformed section of the room temperature leads to a slight decrease in the carbon super-
SENB specimens were ground and polished following conventional saturation of the martensite and resulting in a slight softening of
procedures before measuring the residual austenite content using the steel [23]. The increase in the dislocation density of the steel
the four peak method (two peaks of the ferrite and two peaks of during the cryogenic treatment (plastic deformation due to ther-
the austenite). The parameters employed in these measurements mal stresses), especially during the cooling and the holding stages,
are given in Table 3. It should be noted that the presence of does not result in hardening. This is because it is compensated by
carbides was not considered in a rst approximation. In a second structural relaxation and a decrease in structural distortion due to
approximation, however, the volume fraction of carbides, Vc, the onset of the carbide precipitation which takes place during the
present in every heat treatment was determined by applying heating stage to room temperature.
image analysis to the FEG-SEM micrographs, the retained auste- On the other hand, hardness decreased during the course of
nite content being corrected accordingly. In contrast, the evolution tempering in virtue of carbide precipitation and the subsequent
of the retained austenite content throughout all the processing decrease in the carbon content of the martensite. Nevertheless, the
sequences (samples 1 and 2) was calculated without considering difference between the quenching (Q) and the rst tempering
Table 2
Studied processing sequences: heat treatments (HT) 14 and samples 1-2.
HT1 Austenitizing at 1020 1C for 30 min. followed by gas Triple tempering at 590 1C for 2 h
quench
HT2 Austenitizing at 1020 1C for 30 min. followed by gas Cryogenic treatment at 196 1C for 12 h Triple tempering at 590 1C for 2 h
quench
HT3 Austenitizing at 1020 1C for 30 min. followed by oil Triple tempering at 590 1C for 2 h
quench
HT4 Austenitizing at 1020 1C for 30 min. followed by oil Cryogenic treatment at 196 1C for 12 h Triple tempering at 590 1C for 2 h
quench
Sample 1 Austenitizing at 1020 1C for 30 min. followed by air Cryogenic treatment at 196 1C for 12 h Triple tempering at 590 1C for 2 h
quench (Q) (C) (3 T)
Sample 2 Austenitizing at 1020 1C for 30 min. followed by oil Cryogenic treatment at 196 1C for 12 h Triple tempering at 590 1C for 2 h
quench (Q) (C) (3 T)
Table 3
X-ray diffraction parameters for retained austenite measurement.
Table 4
Tensile properties, Rockwell hardness and fracture toughness of the H13 steel after different heat treatments (HT). Mean values (standard deviation).
a
All the fracture tests comply with the ASTM E1820-09 standard.
contrast, the second and third tempering stages give rise to less
signicant microstructural changes, only the tempering of the
fresh martensite which had been transformed during the cooling
of the rst tempering stage.
Signicant differences were observed, however, in the fracture
toughness results, which are shown in Table 4. HT1 provided the
lowest fracture toughness, whereas HT4 offered the highest value.
The positive effect of the cryogenic treatments is especially worthy
to note. Both HT2 and HT4 respectively gave rise to a 22.5 and a
24% increase compared to their respective treatments without
the cryogenic phase, HT1 and HT3. Moreover, a 41% increase in
fracture toughness was obtained via HT4 compared with HT1. The
quenching medium was also seen to affect the toughness of the
steel due to the effect of the cooling rate, oil being a more severe
quench medium than gas: oil quenching (HT3 and HT4) led to
Fig. 1. Evolution of the Rockwell C hardness (HRC) and the Full Width at Half higher toughness values than gas quenching (HT1 and HT2).
Maximum (FWHM) parameter throughout the overall heat treatment (samples The fracture surface of the SENB specimens constituted an
1 and 2): quenching (Q), cryogenic (C) and tempering (T) stages. important source of information for justifying the obtained results.
SEM analysis, which focused on the onset zone of crack growth
initiation from the fatigue pre-crack, is reported in Fig. 2 (the
stage (Q C 1T) was not notable, 1.3 Rockwell C units for the air bottom of the gures corresponds to the fatigue pre-crack and the
quenching and 3.6 units for oil quenching. This slight variation top, to the crack growth that led to sudden failure of the fracture
may be explained by the transformation of the retained austenite, specimens). Fracture pattern observation revealed the existence
a soft constituent, into martensite, compensating the loss of of a small region where ductile micromechanisms were active
hardness due to the carbon-depleted martensite. Moreover, the (nucleation, growth and coalescence of microcavities) right at the
secondary carbide precipitation, which takes place in tool steels onset of the crack growth. The initial crack blunted and a plastic
during tempering at 500600 1C, also generates an additional zone developed in the crack front before complete failure of the
increase in hardness. The effect of the second and third tempering specimen. Although all the specimens behaved in a brittle way
was even lower. (cleavage fracture), the higher fracture toughness resulting from
Comparing the two heat treatments (air and oil quenching), it the heat treatments provided with a cryogenic stage was directly
can be seen that the hardness values were not very different. linked to the higher plasticity produced in the crack front, this
The evolution of the FWHM parameter throughout the quench- nding being especially relevant after the HT4 treatment, as can be
ing, cryogenic treatment and three tempering stages is also shown seen in Fig. 2d.
in Fig. 1 for air and oil quenching. This parameter was found to
behave identically for both heat treatments. The highest values 3.2. Microstructural analysis
were obtained after the quenching and the cryogenic stages, the
FWHM value subsequently decreasing signicantly during the rst As expected, microstructural analysis of the samples using
tempering. In fact, the FWHM parameter shows an 80% decrease optical microscopy revealed the presence of a tempered marten-
after the rst tempering when quenching in air, and a 90% site microstructure, with ne, spherical, homogeneously dispersed
decrease when quenching in oil. The second and third tempering carbides. In order to justify the fracture toughness results, samples
sequences had practically no inuence on this parameter, as can be were analysed under an FEG-SEM microscope at 100,000 . Fig. 3
seen from Fig. 1. shows the typical carbide pattern of tool steels [10,11]: primary
Fig. 1 also shows that the evolution of the Rockwell hardness carbides, secondary micrometric carbides and secondary nano-
and the FWHM parameter followed the same pattern, although metric carbides.
the decrease in the former during the tempering sequences was It seems clear that carbides precipitated in the course of the
more progressive, while the latter mainly decreased during the HT1 treatment (Fig. 3a) have a relatively coarse and sometimes
rst tempering. As a result of this observation, it may be stated elongated appearance, whereas the HT4 microstructure (Fig. 3d)
that the FWHM is a hardening parameter linked to microstructural shows a more uniform distribution of ner carbides. These results
evolution, as the most representative microstructural changes are in agreement with those reported by other authors [1013] in
are produced during the rst tempering sequence, i.e. the temper- regard to the effect of deep cryogenic treatments on secondary
ing of the quenched martensite (carbide precipitation and carbides: cryogenic treatments produce a ner, homogeneously
decrease in the carbon content of the martensite) and the distributed carbide network and also an increase in the carbide
transformation of the retained austenite into martensite. In volume fraction. Meanwhile, both HT2 and HT3 (Fig. 3b and c) led
36 M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
Fig. 2. Fracture toughness surfaces. Crack growth from the pre-crack: (a) HT1, (b) HT2, (c) HT3 and (d) HT4 (500 ).
to intermediate carbide distributions compared to HT1 and HT4 show a lower retained austenite content than their respective heat
(Fig. 3a and d). treatments without it (HT1 and HT4). Nevertheless, there is a low
The smaller size of the precipitated carbides and their more austenite content that could not be transformed even through the
homogeneous distribution pattern seem to be the reason for the application of the mentioned cryogenic treatments. It is hence
enhanced toughness of the H13 steel as a consequence of the considered not to have any negative effect during the forging
cryogenic treatments, treatment HT4 being the most suitable heat process, as it will not be susceptible to transformation during the
treatment to obtain the highest fracture toughness. service life of the die. Along these same lines, according to Villa
The volume fraction of carbides is shown in Table 5 for heat et al. [24], the application of cryogenic treatments contribute to
treatments 14. As expected, quenched and tempered H13 steel the mechanical stabilization of the retained austenite, avoiding the
has a notable carbide content, up to 10% in every case. The results formation of martensite during the normal service life of dies.
show that cryogenic treatments increased the carbide percentage Fig. 4 gives the results of the retained austenite measurements
of H13 steel 22.3 and a 8.2% when comparing the treatments after each stage of the overall heat treatment (air and oil quench-
without a cryogenic stage (HT1 and HT3) with those that included ing). Firstly, the effect of the quenching medium on the retained
this stage (HT2 and HT4), respectively. Besides, the effect of more austenite content is worth noting. At the end of the quench stage,
severe quenching, such as oil quenching, is similar to the effect of a oil quenching led to lower austenite content than air quenching,
cryogenic stage, resulting in an increase in carbide content of 30% due to the formers higher cooling rate. In fact, the higher retained
between HT1 and HT4. The obtained data are in accordance with austenite content after air quenching is a consequence of the
the KIC fracture toughness; hence, the higher the carbide content, stabilization of the austenite owing to the lower cooling rate.
the higher the toughness, as the carbon content of the martensitic The cryogenic stage modies the residual austenite content,
matrix phase will be lower. especially for air quenching; the reduction being less signicant
The results of the measured retained austenite content (V) for oil quenching. These results are in accordance with the revised
are given in Table 6. For heat treatments 14, these were literature, since a reduction in the retained austenite content is
calculated considering the presence of carbides (Table 5) and usually reported when a cryogenic stage is applied [2429].
without considering their presence. The retained austenite content Tempering was found to be a good way to transform the retained
suffers a slight drop when the volume fraction of carbides is taken austenite into martensite in this steel. In fact, as can be observed in
into account and more precise results are obtained. Fig. 4, the retained austenite fraction decreased to its minimum
In any case, as a result of the triple tempering applied to the value in both the air and oil quenching heat treatments during the
H13 steel, the nal residual austenite content is around or below rst tempering cycle. The application of a second and a third
3%. Those heat treatments with a cryogenic stage (HT2 and HT4) tempering did not provide any further reduction in the austenite
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240 37
Fig. 3. H13 steel microstructure at 100,000 magnication (FEG-SEM): (a) HT1, (b) HT2, (c) HT3 and (d) HT4.
Table 6
Retained austenite content as a function of the heat treatment (HT) and the carbide correction. Volume fraction, % (error, %).
Retained austenite content without carbide correctiona 3.7 ( 71.3) 2.3 ( 7 1.2) 2.9 (7 1.1) 2.5 ( 7 1.0)
Retained austenite content after carbide correctionb 3.3 ( 71.1) 2.0 ( 7 1.0) 2.5 (7 1.0) 2.2 ( 7 1.0)
a
V V 1.
b
V V Vc 1.
Fig. 6. Phase transformations, carbide precipitation and coarsening at each stage of the heat treatment, highlighting the effect of the cryogenic treatment.
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