Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
art ic l e i nf o
a b s t r a c t
Article history:
Received 6 May 2014
Received in revised form
2 October 2014
Accepted 17 November 2014
Available online 25 November 2014
Cryogenic treatments are considered a good way to reduce the retained austenite content and improve
the performance of tool steels. Four different heat treatments, two of which included a deep cryogenic
stage, were applied in this study to an H13 tool steel, subsequently determining its mechanical
properties by means of tensile, hardness and fracture toughness tests. Furthermore, scanning electron
microscopy and X-ray diffraction analysis were performed to gain an insight into the microstructural
evolution of these heat treatments during all the stages.
It was concluded that the application of a deep cryogenic treatment to H13 steel induces higher
thermal stresses and structural defects, producing a dispersed network of ne carbides after the
subsequent tempering stages, which were responsible for a signicant improvement in the fracture
toughness of this steel without modifying other mechanical properties. Although the application of a
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.
Keywords:
AISI H13 tool steel
Deep cryogenic treatments
Mechanical properties
Microstructural evolution
X-ray diffraction
1. Introduction
Traditional hot forging manufacturers are constantly improving
productivity in order to be competitive and maintain or increase their
market share and prots. In this respect, there are three main reasons
why companies are investing to optimize their forging processes: the
gradual increase in energy costs (electricity and gas) in recent years
[1], the competitiveness of rms from emerging countries, and the
development of more economic production technologies with good
mechanical properties, such as modern casting [2].
As a result, forging companies are forced to minimize their
production costs and achieve more efcient processes by means of
the following methods [3]:
Reduction in labour costs via the increased use factory automation systems.
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
2. Experimental methods
2.1. Steel and heat treatments
An H13 steel regularly used to make hot forging dies was
studied in this research. Its chemical composition is given in
Table 1.
Tensile and fracture specimens were subjected to four different
heat treatments involving quenching and tempering. Two quenching media (nitrogen gas and oil) and two types of sequences
(quenching (Q) tempering (T) and quenching (Q) cryogenic
treatment (C) tempering (T)) were carried out. The sequences
and characteristics of the applied treatments can be seen in
Table 2.
Apart from the four sequences described above, an extended
study was conducted to gain an insight into the effects of deep
cryogenic treatments and assess the inuence of the other factors
of the studied heat treatments, such as quenching media and
tempering stages. Two 20 10 8 mm specimens (samples 1
and 2) were cut from the non-deformed central section of the
fracture specimens and were likewise subjected to the heat
treatments described in Table 2. In this case, the effect of quench
severity was studied, comparing oil and air as quenching media.
2.2. Mechanical characterization
The mechanical properties of the H13 steel were measured at
room temperature by means of tensile, hardness and fracture tests.
Tensile tests were performed on cylindrical tensile specimens
of 10 mm diameter with a calibrated length of 70 mm using a MTS
tensile machine equipped with a 250 kN load cell at a displacement rate of 2 mm/min. Three specimens were tested for each
heat treatment. In order to calculate elongation (e), an initial
gage length of 50 mm was considered on each specimen. The
experimental procedure and the determination of the main
Table 1
H13 steel chemical composition (weight%).
%C
%Si
%Mn
%Cr
%Mo
%V
0.39
1.0
0.4
5.2
1.4
0.9
33
parameters were carried out as per the UNE-EN ISO 68921:2009 standard.
The hardness of the steel was determined by means of the
Rockwell C hardness test using a HOYTOM hardness tester under a
load of 150 kg. For treatments HT1 to HT4, samples were extracted
from the non-deformed central section of the SENB specimens
once the fracture toughness test was completed. Five indentations
were made in the thickness direction to appreciate any hardening
due to the cooling rate gradient existing between the surface and
the centre of the samples. Moreover, for samples 1 and 2, Rockwell
C hardness measurements were performed after each stage
(quenching (Q), deep cryogenic treatment (C) and tempering (T))
of the overall heat treatment to appreciate the evolution of
hardness and to compare the results with the Full Width at Half
Maximum (FWHM) parameter, which was obtained in the course
of the X-ray diffraction analysis.
In line with bibliographic references [8,15], KIC fracture toughness tests following the ASTM E1820 standard [16] were carried
out due to the fact that H13 steel is quite brittle at room
temperature. Three single edge notched bend (SENB) specimens,
each with a width (W) of 40 mm, a thickness (B) of 20 mm, a span
(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
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
frequency of 3 Hz and a maximum stress intensity factor, K, of
25 MPa m1/2 in order to prevent sudden fracture of the specimens [15]. The conditional result, KQ, which was determined from
the load versus COD record according to the ASTM E1820 standard,
was consistent with size and linear elastic requirements, so the
results obtained could be considered as material fracture toughness (KIC) [16].
2.3. Fractographic and microstructural characterization
Fractographic and microstructural analyses were carried out to
understand and justify the mechanical testing results. The steel
microstructures were studied by optical and scanning electron
microscopy. The latter technique was also used to characterise the
fracture surfaces.
As far as microstructural examination is concerned, metallographic samples were prepared from the non-deformed central
section of the SENB specimens. These were ground, polished with
diamond paste and nally etched with picral. All samples were
rst observed under a Nikon Epiphot 200 optical microscope and
then, under a FEG-SEM Carl Zeiss GEMINI microscope.
Fracture surfaces from the SENB specimens were likewise
analysed under a JEOL JSM-5600 scanning electron microscope
at different magnications to reveal the predominant failure
micromechanisms. This examination focused mainly on observing
the onset zone of fracture growth from the fatigue pre-crack.
2.4. X-ray diffraction analysis
X-ray diffraction was applied to determine the residual stress
state induced in the heat treatments, the structural distortion, via the
Full Width at Half Maximum (FWHM) parameter, and the retained
austenite content. Measurements were performed for the four
applied heat treatments (HT1HT4), on the non-deformed central
sections of the SENB specimens, as well as on samples 1 and 2.
The FWHM parameter is considered an indicator of the structural distortion of the material. In particular, it is related to the
dislocation density and to the existence of micro-residual stresses
[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
3. Results
3.1. Mechanical properties
The tensile test (elastic modulus (E), yield strength (ys),
ultimate tensile strength (UTS), elongation (e) and area reduction
(Z)) and hardness results are shown in Table 4. The differences
between the four heat treatments were not signicant, HT1 being
affording the highest yield strength and ultimate tensile strength.
Cryogenic treatments did not seem to affect the tensile properties
of the steel. No signicant differences in hardness were observed
between the different heat treatments either.
In addition, the evolution of the average hardness throughout
the overall heat treatment is shown in Fig. 1. It can be seen that the
highest hardness value was obtained after the quenching stage
due to the presence of a non-tempered hard martensite. As it will
be seen later, at the end of the cryogenic stage a certain amount of
retained austenite transforms into martensite, while a slight softening of 0.7 and 0.6 HRC was observed for air and oil quenching,
respectively. It seems that the early carbide precipitation during
the heating stage from the cryogenic temperature ( 196 1C) to
room temperature leads to a slight decrease in the carbon supersaturation of the martensite and resulting in a slight softening of
the steel [23]. The increase in the dislocation density of the steel
during the cryogenic treatment (plastic deformation due to thermal stresses), especially during the cooling and the holding stages,
does not result in hardening. This is because it is compensated by
structural relaxation and a decrease in structural distortion due to
the onset of the carbide precipitation which takes place during the
heating stage to room temperature.
On the other hand, hardness decreased during the course of
tempering in virtue of carbide precipitation and the subsequent
decrease in the carbon content of the martensite. Nevertheless, the
difference between the quenching (Q) and the rst tempering
Table 2
Studied processing sequences: heat treatments (HT) 14 and samples 1-2.
Heat treatments and
samples
Processing sequences
HT1
Austenitizing
quench
Austenitizing
quench
Austenitizing
quench
Austenitizing
quench
HT2
HT3
HT4
Sample 1
Sample 2
Table 3
X-ray diffraction parameters for retained austenite measurement.
Radiation
Cr K
Filter
Austenite measured planes
Ferrite measured planes
Vanadium
(220)
(211)
(200)
(200)
Carbides (%)
0% or Vc
collimator (mm)
Diffraction angles of austenite (2)(1)
Diffraction angles of ferrite (2)(1)
5
130
156.4
80
106.1
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
35
Table 4
Tensile properties, Rockwell hardness and fracture toughness of the H13 steel after different heat treatments (HT). Mean values (standard deviation).
Heat treatment
HT1
E (GPa)
ys (MPa)
UTS (MPa)
e (%)
Z (%)
Hardness (HRC)
KIC fracture toughness (MPam1/2)a
208
1303
1497
16.8
38.8
43.6
54.8
HT2
( 75)
( 75)
( 72)
( 70.9)
( 70.4)
( 71.1)
( 71.7)
210
1265
1469
14.2
41.8
43.6
67.1
HT3
( 7 5)
( 7 9)
( 7 7)
( 7 1.0)
( 7 1.8)
( 7 0.6)
( 7 5.7)
211
1255
1464
12.1
43.4
43.4
62.3
HT4
( 7 6)
( 7 4)
( 7 3)
( 7 1.8)
( 7 1.8)
( 7 0.8)
( 7 1.5)
211
1253
1469
18.0
41.3
43.1
77.4
( 7 3)
( 7 10)
( 7 10)
( 7 1.3)
( 7 2.2)
( 7 1.1)
( 7 6.6)
All the fracture tests comply with the ASTM E1820-09 standard.
Fig. 1. Evolution of the Rockwell C hardness (HRC) and the Full Width at Half
Maximum (FWHM) parameter throughout the overall heat treatment (samples
1 and 2): quenching (Q), cryogenic (C) and tempering (T) stages.
stage (Q C 1T) was not notable, 1.3 Rockwell C units for the air
quenching and 3.6 units for oil quenching. This slight variation
may be explained by the transformation of the retained austenite,
a soft constituent, into martensite, compensating the loss of
hardness due to the carbon-depleted martensite. Moreover, the
secondary carbide precipitation, which takes place in tool steels
during tempering at 500600 1C, also generates an additional
increase in hardness. The effect of the second and third tempering
was even lower.
Comparing the two heat treatments (air and oil quenching), it
can be seen that the hardness values were not very different.
The evolution of the FWHM parameter throughout the quenching, cryogenic treatment and three tempering stages is also shown
in Fig. 1 for air and oil quenching. This parameter was found to
behave identically for both heat treatments. The highest values
were obtained after the quenching and the cryogenic stages, the
FWHM value subsequently decreasing signicantly during the rst
tempering. In fact, the FWHM parameter shows an 80% decrease
after the rst tempering when quenching in air, and a 90%
decrease when quenching in oil. The second and third tempering
sequences had practically no inuence on this parameter, as can be
seen from Fig. 1.
Fig. 1 also shows that the evolution of the Rockwell hardness
and the FWHM parameter followed the same pattern, although
the decrease in the former during the tempering sequences was
more progressive, while the latter mainly decreased during the
rst tempering. As a result of this observation, it may be stated
that the FWHM is a hardening parameter linked to microstructural
evolution, as the most representative microstructural changes
are produced during the rst tempering sequence, i.e. the tempering of the quenched martensite (carbide precipitation and
decrease in the carbon content of the martensite) and the
transformation of the retained austenite into martensite. In
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
higher toughness values than gas quenching (HT1 and HT2).
The fracture surface of the SENB specimens constituted an
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
bottom of the gures corresponds to the fatigue pre-crack and the
top, to the crack growth that led to sudden failure of the fracture
specimens). Fracture pattern observation revealed the existence
of a small region where ductile micromechanisms were active
(nucleation, growth and coalescence of microcavities) right at the
onset of the crack growth. The initial crack blunted and a plastic
zone developed in the crack front before complete failure of the
specimen. Although all the specimens behaved in a brittle way
(cleavage fracture), the higher fracture toughness resulting from
the heat treatments provided with a cryogenic stage was directly
linked to the higher plasticity produced in the crack front, this
nding being especially relevant after the HT4 treatment, as can be
seen in Fig. 2d.
3.2. Microstructural analysis
As expected, microstructural analysis of the samples using
optical microscopy revealed the presence of a tempered martensite microstructure, with ne, spherical, homogeneously dispersed
carbides. In order to justify the fracture toughness results, samples
were analysed under an FEG-SEM microscope at 100,000 . Fig. 3
shows the typical carbide pattern of tool steels [10,11]: primary
carbides, secondary micrometric carbides and secondary nanometric carbides.
It seems clear that carbides precipitated in the course of the
HT1 treatment (Fig. 3a) have a relatively coarse and sometimes
elongated appearance, whereas the HT4 microstructure (Fig. 3d)
shows a more uniform distribution of ner carbides. These results
are in agreement with those reported by other authors [1013] in
regard to the effect of deep cryogenic treatments on secondary
carbides: cryogenic treatments produce a ner, homogeneously
distributed carbide network and also an increase in the carbide
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 ).
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 5
Volume fraction of carbides (%) measured in the different heat treatments (HT).
Heat treatment
HT1
HT2
HT3
HT4
11.2
13.7
13.4
14.5
4. Discussion
Primary vanadium-rich carbides (MC) are expected to be
formed in H13 steel austenitized at a temperature of 1020 1C [8].
Moreover, molybdenum/iron-rich (M6C) and chromium/iron-rich
(M7C3) carbides might also be present due to the application of
low austenitizing temperatures [8]. On the other hand, secondary
micrometric carbides (M7C3) are supposed to form in grain
boundaries during quenching [8,31]. Anyway, deep cryogenic
treatment and tempering do not affect the morphology of coarse
primary and micrometric secondary carbides [10,11], but only
secondary nanocarbides are modied by these heat treatments.
According to many researchers [30,32] and also bearing in
mind the results obtained in this study, a high internal stress state
38
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
Table 6
Retained austenite content as a function of the heat treatment (HT) and the carbide correction. Volume fraction, % (error, %).
Heat treatment
HT1
HT2
HT3
HT4
3.7 ( 71.3)
3.3 ( 71.1)
2.3 ( 7 1.2)
2.0 ( 7 1.0)
2.9 (7 1.1)
2.5 (7 1.0)
2.5 ( 7 1.0)
2.2 ( 7 1.0)
a
b
V V 1.
V V Vc 1.
Fig. 4. Evolution of the retained austenite content (%) throughout the overall heat
treatment (without carbide correction): quenching (Q), cryogenic (C) and tempering (T) stages.
Fig. 5. Evolution of the surface residual stress versus the quenching medium for
each stage of the overall heat treatment (quenching (Q), cryogenic (C) and
tempering (T) stages).
5. Conclusions
The tensile mechanical properties and hardness of an H13 steel
were barely changed in the four applied heat treatments, both the
effect of the quench severity and of the cryogenic treatment being
non-signicant.
Rockwell hardness progressively decreased during the three
tempering stages, whereas the FWHM parameter suffered a
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
39
Fig. 6. Phase transformations, carbide precipitation and coarsening at each stage of the heat treatment, highlighting the effect of the cryogenic treatment.
Acknowledgements
The authors are grateful for the nancial support for this study
provided by CIE Galfor S.A. and the Spanish Ministry of Economy
and Competitiveness, through project CN-12-025-CDTI.
References
[1] EUROFORGE.org [Internet]. Hagen: EUROFORGE; c2014 [cited 2014 Mar 14].
Energy benchmarking. Available from: http://www.euroforge.org/leadmin/
user_upload/Downloads/EUROFORGE_Energy_BM_2012_13.pdf.
[2] W. Menk, L. Kniewallner, S. Prukner, MTZ worldw 68 (5) (2007) 2324.
[3] M. Shirgaokar, Technology to Improve Competitiveness in Warm and Hot
Forging -Increasing Die Life and Material Utilization- (Dissertation), The Ohio
State University, Columbus (OH), 2008.
[4] M. Bayramoglu, H. Polat, N. Geren, J. Mater. Process. Technol. 205 (2008)
394403. http://dx.doi.org/10.1016/j.jmatprotec.2007.11.256.
[5] S. Babu, D. Ribeiro, R. Shivpuri, Material and Surface Engineering For Precision
Forging Dies, Precision Forging Consortium (US), Ohio Aerospace Institute and
National Center for Manufacturing Sciences, 1999 (Final report).
[6] J.R. Davis, ASM Specialty Handbook-Tool Materials, ASM International, Materials Park (OH) (1995) 119153.
[7] R. Shivpuri, in: S.L. Semiatin (Ed.), ASM Metals Handbook, Volume 14, ASM
International, Materials Park (OH), 2005, pp. 4761.
[8] G. Roberts, G. Krauss, R. Kennedy (Eds.), Tool Steels, fth ed.,ASM International, Materials Park (OH), 1998.
[9] C.H. Surberg, P. Stratton, K. Lingenhle, Cryogenics 48 (2008) 4247. http://dx.
doi.org/10.1016/j.cryogenics.2007.10.002.
[10] P. Farina, Efeito das adies de tratamentos criognicos e de alvio de tenses
no ciclo trmico do ao ferramenta (PhD Thesis), University of So Paulo, 2011.
[11] P. Farina, C. Barbosa, H. Goldenstein, Proceedings of the 18th IFHTSE Congress
(2010) 54175426.
[12] P. Farina, A. Farina, C. Barbosa, H. Goldenstein, Tecnol. Metal. Mater. Miner 9
(2) (2012) 140147.
[13] M. Pellizzari, A. Molinari, S. Gialanella, G. Straffelini, Metall. Italiana 93 (1)
(2001) 2127.
[14] P. Baldissera, C. Delprete, Open Mech. Eng. J. 2 (2008) 111.
[15] J.C. Bergeron, E. Burns, J. Bushie, H. Sandberg, A.V. Heuvel, A. Carrico, Failure
Analysis of H13 Gear Blank Forging Dies (Final report), Michigan Technological
University, Houghton (MI), 2004.
[16] ASTM E 1820-09. Standard Test Method for Measurement of Fracture Toughness, American Society for Testing and Materials.
[17] I.C. Noyan, J.B. Cohen, Residual stress: measurement by diffraction and
interpretation, Springer, New York, 1987.
[18] A.T. Vielma, Parmetros de shot peening y sus efectos en el comportamiento a
fatiga del acero F1272 (PhD Thesis), University of Oviedo, 2013.
[19] I. Fernndez-Pariente, S. Bagherifard, M. Guagliano, R. Ghelichi, Eng. Fract.
Mech. 103 (2013) 29. http://dx.doi.org/10.1016/j.engfracmech.2012.09.014.
[20] M.E. Fitzpatrick, A.T. Fry, P. Holdway, F.A. Kandil, J. Shackleton, L. Suominen,
Measurement Good Practice Guide No. 52.Determination of residual stresses
by X-ray diffraction Issue 2 (Report), National Physical Laboratory, Teddington (UK), 2005.
[21] P.S. Prevey, in: ninth ed.,in: R.E. Whan (Ed.), ASM Metals Handbook, Volume
10, ASM International, Materials Park (OH), 1986, pp. 380392.
[22] Software user's guide, preliminary. Finland: Stresstech Oy, 2010.
[23] D. Das, A.K. Dutta, K.K. Ray, Mater. Sci. Eng. A 527 (2010) 21822193. http://dx.
doi.org/10.1016/j.msea.2009.10.070.
40
M. Prez, F.J. Belzunce / Materials Science & Engineering A 624 (2015) 3240
[24] M. Villa, K. Pantleon, M.A.J. Somers, Acta Mater. 65 (2014) 383392. http://dx.
doi.org/10.1016/j.actamat.2013.11.007.
[25] A. Bensely, S. Venkatesh, D. Mohan Lal, G. Nagarajan, A. Rajadurai, K. Junik, Mater.
Sci. Eng. A 479 (2008) 229235. http://dx.doi.org/10.1016/j.msea.2007.07.035.
[26] M. Preciado, M. Pellizzari, J. Mater. Sci. 49 (2014) 81838191. http://dx.doi.org/
10.1007/s10853-014-8527-2.
[27] S. Li, Y. Xie, X. Wu, Cryogenics 50 (2010) 8992. http://dx.doi.org/10.1016/j.
cryogenics.2009.12.005.
[28] A.I. Tyshchenko, W. Theisen, A. Oppenkowski, S. Siebert, O.N. Razumov, A.
P. Skoblik, et al., Mater. Sci. Eng. A 527 (2010) 70277039. http://dx.doi.org/
10.1016/j.msea.2010.07.056.
[29] D. Yun, L. Xiaoping, X. Hongshen, Heat Treat. Met. 25 (3) (1998) 5559.
[30] D. Senthilkumar, I. Rajendran, M. Pellizzari, J. Siiriainen, J. Mater. Process.
Technol. 211 (2011) 396401. http://dx.doi.org/10.1016/j.jmatprotec.2010.10.018.