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JMEPEG (2016) 25:1041–1046 ASM International

DOI: 10.1007/s11665-016-1895-9 1059-9495/$19.00

Hot Ductility of the 17-4 PH Stainless Steels


V. Herrera Lara, L. Guerra Fuentes, O. Covarrubias Alvarado, A. Salinas Rodriguez, and E. Garcia Sanchez

(Submitted May 5, 2015; in revised form December 24, 2015; published online January 21, 2016)

The mechanisms of loss of hot ductility and the mechanical behavior of 17-4 PH alloys were investigated
using hot tensile testing at temperatures between 700 and 1100 °C and strain rates of 1024, 1022, and
1021 s21. Scanning electron microscopy was used in conjunction with the results of the tensile tests to find
the temperature region of loss of ductility and correlate it with cracking observed during processing by hot
upsetting prior to ring rolling. It is reported that 17-4 PH alloys lose ductility in a temperature range
around 900 °C near to the duplex austenite + ferrite phase field. Furthermore, it is found that niobium
carbides precipitated at austenite/ferrite interfaces and grain boundaries have a pronounced effect on the
mechanical behavior of the alloy during high-temperature deformation.

in solid solution may also have detrimental effects on hot


Keywords 17-4 PH, ductility trough, hot cracking, hot ductility,
hot tensile tests, mechanical behavior ductility, for example, Cu and Sn promote loss of ductility (Ref
9, 14). In steels containing large amounts of C, Al, and Nb, the
ductility is degraded when the steel also contains P (Ref 15,
16). The high-temperature ductility of steels with large amounts
of Si is affected negatively near 1050 C due to the formation
1. Introduction of Si-Fe oxides (Ref 11).
The 17-4 PH alloy is used for the manufacture of seamless
rings by hot forging. However, hot cracking can occur during
Precipitation hardening steels may be used as an alternative
one-step upsetting leading to the entire scraping of the material.
material when normal stainless steels cannot provide adequate
Actually, there is very limited information regarding the loss of
strength and toughness for service conditions at relatively high
ductility in these steels; consequently in this paper, the effects
temperatures. The 17-4 PH is one of the most popular steels
of steel composition, deformation temperature, and strain rate
used in a wide range of industrial applications. Its ability to
on the hot ductility of 17-4 PH stainless steel, as estimated from
develop very high strength without undue loss of ductility and
measurements of reduction of area at fracture during hot tensile
its superior corrosion resistance in comparison with other steels
tests, are presented and discussed in terms of their microstruc-
of similar strength have made it a very attractive material (Ref
ture before and after hot testing. This is expected to contribute
1, 2). However, under certain processing conditions, loss of
to the understanding of the causes of loss of ductility in 17-4
ductility has been observed and there is not a unique
PH during high-temperature deformation.
mechanism to explain this behavior (Ref 3).
The study of hot ductility of metals is of relevance for
industrial processes such as hot rolling, ring hot rolling, hot
forging, etc. The loss of hot ductility is a serious problem 2. Experimental Procedure
during forging of high-alloy steels. Several mechanisms have
been associated with cracking during the hot forging of low- 17-4 PH steels were obtained from two different suppliers;
alloy steels (Ref 3-7). However, just a few investigations have samples of both steels were obtained directly from forged bars.
been reported on the hot working behavior of 17-4 PH alloy Materials are identified as E (Vacuum arc re-melting) and U
(Ref 1, 2, 8). The hot ductility loss at relatively low (Electro-slag re-melting), respectively. The materials were
temperatures in low carbon advanced high-strength steels is machined to produce standard tensile test specimens,
associated with microvoid nucleation, growth, and coalescence 25.4 mm in diameter and 76.2 mm in length, with tensile axes
at precipitates and/or inclusions, particularly MnS (Ref 9, 10), parallel to the usual forging direction. Initial microstructure and
CuS, V(C, N), and AlN (Ref 11, 12), which play an important Vickers microhardness were measured and compared. The test
role on the crack nucleation mechanism (Ref 4, 13). Elements specimens were sectioned after tensile testing, mounted,
ground, and polished using standard metallographic technics.
The microstructure was characterized after etching the surfaces
V. Herrera Lara, L. Guerra Fuentes, and E. Garcia Sanchez,
with Gliceregia (60% HCl, 20% HNO3, and 40% glycerol)
Universidad Autónoma de Nuevo León, FIME-CIDET, Av.
Universidad s/n. Cd. Universitaria, San Nicolás de los Garza, NL, during 30 s. Microhardness values were obtained using a 500 g
México, C.P. 66451; O. Covarrubias Alvarado, Universidad load by 20 s. Table 1 shows the chemical composition of the
Autónoma de Nuevo León, FIME-CIDET, Av. Universidad s/n. Cd. steels and the nominal composition of 17-4 PH.
Universitaria, San Nicolás de los Garza, NL, México, C.P. 66451, and Hot tensile test was performed at temperatures from 700 to
Exova, Monterrey, N. L., México, C.P 66367; A. Salinas Rodriguez, 1100 C and at initial strain rates of 10 4, 10 2, and 10 1. All
Centro de Investigacióny de Estudios Avanzados del IPN tests were carried out under an atmosphere produced by flowing
(CINVESTAV), Unidad Saltillo Carretera Saltillo-Monterrey km
13.5, Ramos Arizpe, Coahuila, México, C.P. 25000. Contact e-mail: Ar to reduce the oxidation of the samples during the tests. After
egs7710@gmail.com. fracture, percentage area reduction (%RA) measurements were

Journal of Materials Engineering and Performance Volume 25(3) March 2016—1041


performed using stereoscopic and secondary electron SEM in prior austenite grain size, steel U was heat treated at a higher
images from the fracture surfaces (Fig. 1). In addition, temperature prior to cooling to room temperature. Despite these
longitudinal sections obtained from the tensile samples were microstructural differences, the average hardness values for
polished and characterized by SEM to investigate microstruc- steels E and U were similar, 32.4 Rc and 33.7 Rc, respectively.
tural details and the nature of the failure mechanisms. Figure 3 shows the dilatometric curves for steels E and U
obtained using a heating rate of 10 C/min. As can be seen, the
transformation to austenite on heating starts at Ac1 = 681.9 C
and finishes at Ac3 = 739 C for steel E. These temperatures
3. Results and Discussion are slightly higher for steel U, Ac1 = 698.1 C and
Ac3 = 749.4 C. Ms temperatures were calculated from the
Figure 2 shows a comparison between the microstructures chemical composition using the AndrewÕs equation (Ref 17)),
of steels E and U in the as-received condition. Ms (C) = 539 423(%C) 30.4(%Mn) 17.7(%Ni) 12.1
As can be observed, the microstructure of both steels (E and (%Cr) 7.5(%Mo). This equation gives the Ms temperature
U) consists of the d-ferrite islands and stringers in a martensitic of steel E as 286 C and of U steel as 284 C. From these
matrix. Quantitative estimation by image analysis techniques results, it is clear that the tensile tests performed in the
showed that the d-ferrite content in steel U (3.16%) is about 2.5 present investigation were carried out at temperatures within
larger than that observed in steel E (1.12%). In addition, the the range of stability of the austenite phase (except the test
sizes of the d-ferrite islands, stringers, and the martensite performed at 700 C).
packets and blocks are larger in steel U than in steel E. This last The maximum strength obtained in tensile tests depends of
observation indicates that the austenite grain size from which many factors; the most important are the strain rate and
they were produced was larger in steel U than in steel E. deformation temperature. Figure 4 illustrates the effects of
According to Table 1, the potential for d-ferrite formation strain rate and temperature of deformation on the maximum
during solidification (Ni and Cr equivalents) is quite similar for tensile strength of steels E and U. As can be seen, the general
both steels. Using the Schaeffler-DeLong diagram with Ni and trends are similar, the maximum tensile strength increases as
Cr equivalents of 8.2 and 16.5, respectively, a microstructure the strain rate increases and the deformation temperature
consisting of martensite with approximately 5-10% d-ferrite is decreases. Increasing the strain rate causes a significant
predicted. It appears then that the as-received materials are in reduction of the time needed for microvoid nucleation during
the solution-treated condition and, considering the differences tension and dynamic precipitation of carbides and nitrides; on

Table 1 Chemical composition of the experimental steels


C Cr Ni Cu Nb Mn S P

E (vacuum arc re-melting) 0.045 15.45 4.59 3.33 0.33 0.29 0.001 0.022
U (electro-slag re-melting) 0.028 15.69 4.36 3.27 0.28 0.79 0.003 0.019
Nominal (Min-Max). 0.070 15.5 3.00 3.00 0.15 1.00 0.030 0.040
17-5 5.00 5.00 0.45

Si Mo Co V Ti Al N Sn

0.49 0.23 0.15 0.05 0.01 <0.01 0.013 0.005


0.27 0.17 <0.05 0.08 <0.01 <0.01 0.035 0.0085
1.0 … … … … … … …

Fig. 1 (a) SEM and (b) stereographic images used to measure the diameter of the fracture surfaces for the estimation of %RA after tensile test-
ing. Comparative measurement

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Fig. 2 Photomicrographs of the microstructures of a longitudinal section of (a) steel E and (b) steel U

Fig. 3 Ac1 and Ac3 transformation temperatures for steels E and U


Fig. 4 Effect of strain rate on the maximum tensile strength at dif-
determined by dilatometry
ferent deformation temperatures for the steels E and U

the other hand, increasing the deformation, thermally activated tested. As can be seen, the r-T curve corresponding to the strain
strain-producing mechanisms promote the plastic flow and rate of 10 4 s 1 exhibits a ‘‘hump’’ centered precisely at
tensile strength reduction, modifications in this behavior are 900 C. This type of behavior has been reported for some
normally related with the changes in the active deformation stainless steels as a manifestation of dynamic aging and, in
mechanisms (Ref 18). general, this phenomenon disappears with increasing strain rate
The slope of the r- e_ curves also depends on temperature as (Ref 19). In the present steels, it appears that dynamic
shown in Fig. 4. There is a rapid decrease in the strain rate precipitation in austenite during deformation may lead to the
dependence of the strength as the temperature increases. It is strength ‘‘hump’’ observed in the r-T relationship as illustrated
also possible to observe major data dispersion in temperatures in Fig. 5.
below 900 C, it could be because of the results of the Therefore, the flow strength ‘‘hump’’ and the ductility
dilatometric tests presented in Fig. 3, below this temperature, minimum observed in steel U could be evidence of a change in
the microstructure is composed by austenite and d-ferrite, and is the deformation mechanism normally associated with phase
not possible to separate the contributions of each phase in the transformations (Ref 20).
mechanical response of the steel. At temperatures of 900 C The most effective method to evaluate the ductility of metals
and above, deformations were carried out in the fully austenite by means of high-temperature tensile testing uses measure-
region and at this temperature, it is noteworthy that the ments of percentage of area reduction (%RA) after fracture.
minimum slope of r- e_ straight lines is reached. In general, the Figure 6 illustrates the effects of strain rate on the %RA-T
decrease in the rate of change of tensile strength with the relationship for the steels E and U. As can be observed, steel U
increase of the deformation temperature may be associated with exhibits ductility troughs for all the strain rates tested, while
increased stability in tension and with the increase in the rate at steel E only exhibits a ductility trough at 10 4 s 1. In the case
which thermally assisted dynamic recovery mechanisms can of steel E tested at higher strain rates, the ductility increases as
take place. temperature increases. The ductility minima observed in the
Figure 5 illustrates the effects of deformation temperature data for steel U take place at about 900 C for strain rates of
on the maximum tensile strength for each of the strain rates 10 4 and 10 2 s 1, in the single-phase austenite region in

Journal of Materials Engineering and Performance Volume 25(3) March 2016—1043


Fig. 5 Effect temperature on the maximum strength in the steels E and U

Fig. 6 Hot ductility curves for the 17-4 PH steel

accordance with the dilatometric studies and occur at 1000 C region, since the ferrite layers have an overriding effect when
for testing at a strain rate of 10 1 s 1. It is also noteworthy that austenite and ferrite coexist. It has been shown that the
the %RA at the ductility minimum decreases significantly as coarsening of precipitates is quite effective in improving the hot
the strain rate decreases. Although a ductility minimum is ductility of various steels (Ref 21).
observed for steel E tested at 900 C and 10 4 s 1, the values Increasing the C content in the steel moves the ductility
of %RA for all testing conditions were all superior to 80%. trough to lower temperatures due to the decrease in the Ac3
Therefore, the mechanisms of ductility loss active in steel U do temperature. This effect affects the starting point of the
not appear to take place in steel E and this material keeps its decrease in hot ductility and has been observed when the
high ductility for all the different conditions evaluated. The carbon content increases in the range of 0.06 and 0.1 wt.%
ductility reduction in this steel tested at 10 2 and 10 1 s 1 can (Ref 22). In the materials used in the present investigation, the
be associated solely with the decrease in testing temperature difference in C contents is 0.017 wt.% and apparently does not
(Ref 11). affect the position of the ductility minima when testing is
As shown in Fig. 7(a) and (b), the initial (prior to performed at a strain rate of 10 4 s 1.
deformation) microstructure of steel U exhibits small particles The mechanisms of loss of ductility at elevated temperature
at d-ferrite/martensite interfaces. EDS (Fig. 7c and d) analysis have been reported by Mintz et al. (Ref 18); all these
of these particles showed evidence of the presence of Nb. The mechanisms can affect the ductility behavior in a synergistic
effect of the presence of fine Nb(C,N) precipitates on the manner depending on the processing conditions and microstruc-
ductility is more pronounced when the test temperature is in the tural characteristics of the steel (Ref 3, 18, 23). In the case of the
low austenite region rather than at the austenite plus ferrite 17-4 PH steel investigated in the present work, the observed loss

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Fig. 7 (a,b) Particles and microvoids near to the fracture surface in a polished longitudinal section. (c,d) EDS analysis

of ductility at temperatures above A3 could be associated with plasticity (Ref 18, 28), the amount of N should be reduced as
the formation of precipitate-free zones (PFZ) in the grain low as possible to avoid cracking (Ref 28). Also has been
boundaries of austenite, and below of A3 (c + d-ferrite) could be reported the combined effect of Nb with other alloying
related with development of strain concentration at the austenite/ elements, and in most of the cases it reduce hot ductility
d-ferrite interfaces and microvoid nucleation, growth, and during deformation (Ref 16, 25).
coalescence; it is due to the difference in ductility between Increasing the strain rate improves the hot ductility, in both
these phases and the presence of Nb-rich precipitates. These steels in spite of the evident low ductility observed in the steel
precipitates similar to AlN (Ref 11, 24) and others (Ref 4, 25) U. This effect has been related with the reduced time for the
promote the nucleation of microvoids during the deformation formation and diffusion-controlled growth of voids around the
and finally their growth and coalescence generating cracking precipitates in the grain boundaries and interfaces (Ref 18).
and fracture (Ref 11). Additionally, it has been reported that
decreasing the strain rate during high-temperature deformation
increases the amount of precipitates (Ref 26). Also the Nb(C,N)
precipitation is affected by deformation and cooling rate, and 4. Conclusions
has been reported dynamic precipitation and more detrimental
effect during high-cooling rates (Ref 13, 27). Additionally, the Under the testing conditions, the 17-4 PH steel showed a
precipitation of Nb(C, N) can be performed dynamically and is decrease in the ductility, starting over the region of Ac3. This is
more extensive in these steels. Solution temperature in Nb steels associated with the difference in the resistance of each phase,
has been reported to be about 1100 C; however, this temper- and the concentration of the strain in more ductile regions of d-
ature also coarsens the precipitates without taking any signif- ferrite and their interaction with the precipitates in the
icant volume fraction back to solution (Ref 18). interphases. This behavior was observed in the steel with
The amount of N is higher in the steel U (0.035%) and major amount of N and reduced level of C. The steel with lower
consequently the amount of precipitates is superior and the levels of N and consequently low amount of Nb(C, N)
ductility reduced in all different conditions of evaluation. presented high ductility in the range of temperatures evaluated
Finally, the effect of Nb(C, N) on the hot ductility depends of (700-1100 C) and in the range of strain rates. The worst
the chemical composition. For 0.015%Nb increasing the ductility was observed in the austenitic region about 900 C to
amount of N from 0.002 to 0.006% markedly reduces the 10 4 s 1 and 1000 C in samples deformed at 10 1 s 1.

Journal of Materials Engineering and Performance Volume 25(3) March 2016—1045


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