AISI 4340 HSLA Under Quenched and Tempered Conditions PDF
AISI 4340 HSLA Under Quenched and Tempered Conditions PDF
Abstract
In this work, the mechanical properties and microstructures of AISI 4340 high strength alloy steel under different tempering
conditions are investigated. The specimens are quenched and tempered to a martensite structure and loaded to fracture at a
constant strain-rate of 3.3 ×10 − 4 s − 1 by means of a dynamic material testing machine (MTS 810). The mechanical properties and
strain-hardening exponent are considered as function of the tempering conditions. The morphological features of the as-quenched
martensite and their evolution during tempering are described. Fractographs of the specimens are also made in order to analyse
their fracture and embrittlement mechanisms. The results indicate that the mechanical properties and microstructural features are
affected significantly by tempering temperature and holding time. The strength and hardness of tempered martensite drop as the
tempering temperature and holding time are increased. However, the ductility increases with increasing tempering temperature and
holding time, except when tempered martensite embrittlement occurs. Microstructural observations reveal that the carbide
precipitates have a plate-like structure at low temperatures, but are spheroid-like at high temperatures. Under the tested
conditions, the fracture appearances show that the material failed in a ductile manner except for the case of tempering at 300°C,
where tempering martensite embrittlement occurs due to the existence of retained interlath austenite. © 1999 Elsevier Science S.A.
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W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206 199
Table 1
Chemical analysis of AISI 4340 alloy steel
Elements C Si Mn Ni Cr Mo P S
Therefore, from the commercial point of view, the However, their concentration is reduced considerably
study of martensitic steels have to include that of steels by the vacuum arc remelt (VAR) process [12]. For the
tempered in the range of 200 – 250°C. present tests, in order to obtain different quenched-and-
However, apart from the effect of tempering temper- tempered martensite structures, samples from the as-re-
ature, the strength of the martensitic structure is domi- ceived steel are firstly austenitised at 850°C for 30 min,
nated by the carbon content and the (Ms –Mf) followed by oil cooling to produce a quenched marten-
temperature range [9,10]. In the case of low-carbon site structure, and then tempered at 100, 200, 250, 300,
martensite, the martensite units form in the shape of 400, 500 and 650°C, for 2 and 48 h, respectively. After
lath, grouped into larger sheaves or packets. Its sub- heat treatment, cylindrical tensile specimens are ma-
structure consists of high densities of dislocations ar- chined in the longitudinal orientation from the extruded
ranged in cells, and is superficially similar to that bar. The size and geometry of the specimens as well as
developed in iron by a heavy cold-working process. In the testing procedure are in accordance with ASTM
the case of high-carbon steels and iron alloys with Ms standard E 8 (1981) for tension testing. Under this
below the ambient, their structure is plate martensite, standard a nominal gauge length of 50 mm and a gauge
which consists of very fine twins with a spacing of of 12.5 mm are utilised in preparing the specimens.
about 50 Å. Their crystal structure may be either (bct) For mechanical tests, the specimens are mounted on
or (bcc). However, in the case of medium-carbon steels, a dynamic material testing system (MTS) and pulled to
since they may contain a mixture of lath and plate fracture at room temperature with a constant cross-
martensite, their structure is more complicated. These head speed of 0.0083 mm s − 1, which corresponds to an
results also indicate that the mechanical behaviour of a initial strain rate of 3.3× 10 − 4 s − 1 (if all the crosshead
quenched-and-tempered steel depends strongly on its movement is transmitted to the specimen), in order to
microstructure. Thus, the study of effects of the mi- obtain the room temperature flow properties. A strain-
crostructure and dislocation structure of a steel on its gage extensometer with a nominal gauge length of 25
strength, ductility and fracture characteristics is of great mm is utilised to measure the deformation of the speci-
importance from the viewpoint of both theory and mens and the cross-head motion relative to the central
practice. pull-bar. The mechanical properties, such as ultimate
Although AISI 4340 steel is a widely-used low-alloy tensile strength, yield strength, and percentage reduc-
martensitic steel that provides an advantageous combi- tion area, are calculated from the stress–strain dia-
nation of strength, ductility and toughness for the grams obtained from the tensile testing, in which the
applications of machine part-members, it is susceptible latter three specimens under identical conditions are
to embrittlement during the tempering procedure within used.
a specified temperature range. In order to prevent this After mechanical testing, the specimens for transmis-
fault, a study on the microstructure and mechanical sion electron microscopy (TEM) observation are cut
properties of AISI 4340 steel under different tempering from the fractured tensile halves by a spark cutting
conditions becomes necessary, these questions being machine, first into slices of approximate 0.25 mm thick-
focused on in this study. Further, the behaviour of ness, and second into discs of 3 mm diameter. The
tempered embrittlement as well as its formation mecha- 3-mm discs are then ground with no. 600 emery paper
nisms are also described. to thickness appropriate for jet thinning and afterwards
electropolished with a jet thinning instrument (Tenupol
3, Struers, double jets) in solution of 5% perchloric acid
2. Material and experimental details and 95% acetic acid (by volume) maintained at 0°C
with a voltage of 20–30 V, until the discs are perfo-
AISI 4340 high-strength alloy steel, supplied in the rated. Jet thinning is carried out on both faces of the
form of an extruded bar of 25.4 mm diameter, is used discs to reduce their thickness at the centre. To prevent
in this study, its chemical composition being given in the perforation from being damaged by force of the jet,
Table 1. AISI 4340 steel is a low-alloy martensitic steel jet thinning has to be discontinued when the samples
that can be heat treated to provide a wide range of are nearly perforated, then a window technique is used
hardness values. Other studies have shown that most of to perforate these samples delicately. The thin foil
the inclusions in AISI 4340 steel are MnS particles [11]. specimens are then examined with a Jeol 2000FX elec-
200 W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206
Table 2
The mechanical properties of AISI 4340 alloy steel after 2 h tempering
Tempering temperature (°C) 100 200 250 300 400 500 650 Quenching
tron microscope operating at 200 kV to reveal the increased, however, the effect of tempering temperature
dislocation substructure and the precipitation of is more significant than that of holding time. Fig. 3
carbides. shows that tested samples’ area reduction and elonga-
Following the mechanical testing, the observations of tion varied with the tempering temperature and holding
the fracture surface for each fractured tensile specimen time. It is clear that the ductility of material increases
are also conducted. Sections of the fracture surface are with the tempering temperature and holding time, but
removed from the fractured tensile bar and then treated that there is then a drop in toughness and ductility
with standard metallographic procedures for micro- when tempered at 300°C.
scopic examination. The observation of the topographi- It has been known for many years that high strength
cal features is carried out using a Jeol JX A-840 martensitic steel heat-treated to achieve the optimum
scanning electron microscope operated at 2.5 kV. combination of strength, ductility and toughness may
result primarily from different processes of heat temper-
ing. This loss in toughness may result primarily from
3. Results and discussion different processes of heat treatment. Actually, in the
as-quenched state, the thermal instability of interlath
3.1. Effects of tempering temperature and holding time austenite after tempering often leads to the formation
on the mechanical properties of carbide films, which is a fairly general cause of
tempered martensite embrittlement. As for the present
case, a loss in toughness after tempering at 300°C is
The mechanical properties, i.e. ultimate and yield
correlated with the retained interlath austenite and the
strengths, hardness, reduction in area, elongation, and
formation of interlath carbide films that are decom-
strain-hardening exponent n, are measured as functions
posed from the lath boundary retained austenite. The
of tempering temperature and holding time. For every
phenomena and possible mechanisms of embrittlement
measurement, three specimens are used, having been
will be described in detail hereinafter in Section 3.3.
quenched (850°C/30 min) in oil and tempered at 100,
200, 250, 300, 400, 500 and 650°C, for 2 and 48 h,
3.2. Measurement of the strain-hardening exponent
respectively. The results obtained are listed in Tables 2
and 3, in which the data for the as-quenched condition The true stress–strain curves for AISI 4340 steel
are included for comparison. As expected, the mechani- conform closely to Ludwik’s relationship s=Ko n,
cal behaviour of AISI 4340 steel is quite sensitive to the where K is the strength coefficient and n is the strain-
tempering temperature and holding time. Under as- hardening exponent. These two constants describe com-
quenched conditions, the material has the highest level pletely the shape of the true stress–strain curves. The
of strength and hardness, but its ductility is the lowest. value of ‘K’ provides some indication of the level of
This can be explained based on the phase transforma- strength of the material and of the magnitude of forces
tion of steel during quenching processes, where the required in forming, whilst the value of ‘n’ correlates
lattice structure of steel changes immediately from a the slope of the true stress–strain curve, i.e. the rate of
face-centred cubic (g phase) to a body-centred tetrago- work hardening, which provides a measure of the abil-
nal (martensite). At the same time, a large amount of ity of the material to retard localization of deformation.
distortion occurred during the formation of the In uniaxial tension, the equivalent stress si equals the
platelets of martensite, which leads to rapid increase of tensile stress s, and the equivalent strain oi equals the
strength and hardness. tensile strain o, consequently the true stress–strain
For the tempering case, the variations of strength curve is the same as the curve s =Ko n. The stress s
and hardness of the AISI 4340 steel with tempering must not be greater than the tensile instability stress
temperature and holding time are shown in Figs. 1 and scrit which corresponds to the maximum load in simple
2, and indicate that the strength and hardness decrease tension and in turn marks the end of uniform straining,
as the tempering temperature and holding time are thus scrit = K(ocrit)n.
W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206 201
Table 3
The mechanical properties of AISI 4340 alloy steel after 48 h tempering
Tempering temperature (°C) 100 200 250 300 400 500 650 Quenching
When the ultimate tensile stress is exceeded, deforma- which the very high strength maraging steels are in-
tion becomes localised to the necked region of the cluded. Rosenfield and Hahn’s data not only confirm
specimen and the material within this region is no the general conclusion of Hollomon and Zener [14] but
longer subject to a purely uniaxial tensile stress but a also show that a linear relationship exists between the
complicated system of triaxial tensile with shear stress, yield stress and the strain-hardening exponent, which
in which the maximum stress occurs at the centre of the demonstrated that for the properties of steel a high
necked region. This phenomenon has been described in strength cannot coexist with high work hardening.
detail by Wigley [13]. According to the definition of the Therefore, it is not easy to obtain both a high strength
strain-hardening exponent for pure tension as men- and a high rate of work hardening in the same class of
tioned above, the values of n are determined and sum- steel.
marised in Tables 2 and 3, from which it can be found
that the value of n decreases rapidly with increase of the 3.3. The effects of tempering temperature and holding
tempering temperature for both cases of 2 and 48 h, time on the fracture beha6iour and embrittlement
and that the values of the strain-hardening exponent n mechanisms
are shown to be a linear function of the yield strength,
as shown in Fig. 4. This result indicates that under all Microscopic observations were made at the fracture
the present conditions, the deformation of the AISI surface to help to identify quantitatively the mode of
4340 steel is dominated by the mechanism, i.e. a ther- fracture initiation as a function of tempering tempera-
mally activated mechanism, and that the rate of dislo- ture. For all of the specimens tested, the observation of
cation annihilation is also the same for each increment the fracture surface shows that heavy necking has taken
of tempering temperature. Hollomon and Zener [14] place during tensile loading. The typical ductile ‘cup-
indicate that in a wide variety of steels the product of and-cone’ fracture surface includes three parts: the fibre
the yield stress and strain-hardening exponent is found region in the centre; the outside smaller shear lip; and
to be a constant, f, having a value in the range of the larger radial region between the two. An example of
8000 –16000 psi (79 – 158 MPa). Rosenfield and Hahn these features is shown in Fig. 5, which corresponds to
[15] made a similar analysis by incorporating their that for specimens tempered at 100°C. It should be
results of line-pipe steel with those of other studies in noted here that, in the as-quenched condition, although
some voids appears on the fracture surface, the frac-
Fig. 4. Effect of the yield stress on the strain-hardening exponent of Fig. 6. Fractograph of an AISI 4340 steel specimen, as quenched in
AISI 4340 steel. oil (850°C/30 min).
W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206 203
Fig. 7. Fractograph of specimen quenched in oil (850°C/30 min) and Fig. 9. Fractograph of specimen quenched in oil (850°C/30 min) and
tempered at 200°C for 2 h. tempered at 300°C for 2 h.
the lath boundary. The orientation relationship be- changes and the dislocation distribution under the vari-
tween a-ferrite and retained austenite satisfies the K–S ous tempering processes employed.
relation. Therefore, we can conclude that the lath
boundary retained austenite decomposes to form car- 3.4.1. Structure of the as-quenched martensite of AISI
bide films cementite should be responsible for the tem- 4340 steel
pered martensite embrittlement of AISI 4340 steel The morphology of martensites (Fig. 12 (optical mi-
under presented testing condition. croscope) and Fig. 13 (electron transmission micro-
When specimens were tempered at the higher temper- scope)), consists mostly of dislocated martensite laths.
ature of 650°C (Fig. 11), although their fracture fea- Isolated examples of internal twins are also seen in a
tures slightly differ from that observed in the lower few plates. Generally, the laths, about 0.5 microns wide,
tempered conditions (500°C), their fracture mode is are separated by low angle boundaries and each
still dominated by the transgranular microvoid coales- martensite lath is composed of many dislocation cells.
cence. In this condition, the appearance of the fracture Since Ms of AISI 4340 steel is above room tempera-
surface consists of two types of dimples. The larger ture, this leads to an autotempering behaviour in the
ones may result from carbide precipitates and the as-quenched structure, thus in the case of quenched
smaller ones are ascribed to characteristics of the martensite there are some brief periods in which carbon
material. atoms can redistribute themselves. Because the stress
fields in lath martensite are situated around individual
3.4. The 6ariations of microstructure with tempering dislocations and cell walls, certain interstitial lattice
temperature and holding time sites near to these places, seen as defected ones, provide
lower energy for carbon than the normal sites. Such
Thin foils of this martensitic steel are studied in detail migration can be detected by metallography or by a
with TEM to realise the nature of the structural smaller contribution of carbon to electrical resistivity or
to internal friction, if comparing the carbon situated in
an interstitial site near to a dislocation with that in a
‘normal’ one [16]. Autotempered precipitates are not
present in any of the twinned plates but are only
resolved in the dislocated laths and untwinned plates.
This suggests strongly that dislocated laths and un-
twinned plates form first near to Ms, whilst twinned
plates forms at lower temperatures, i.e. near to Mf.
Fig. 10. Structure of the martensite of AISI 4340 alloy steel tempered
at 300°C: (a) DF using one austenite reflection; (b) SADP; and (c) Fig. 12. OM micrograph of the as-quenched martensite of the AISI
indexing of (b). 4340 steel (quenched in oil, 850°C/30 min).
W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206 205
Fig. 13. TEM micrograph of the AISI 4340 steel as-quenched lath Fig. 15. TEM micrograph of a specimen quenched in oil (850°C/30
martensite. min) and tempered at 200°C for 48 h.
Growth of the precipitated carbide with tempering tallisation yields a rapid decrease of the dislocation
holding time can also be seen. density and internal strains.
When the quenched structure of AISI 4340 steel is It should be noted that when the quenched struc-
tempered at high temperature, i.e. 650°C for 2 h, the ture is tempered at high temperature, reaching 650°C,
microstructure consists of equiaxed grain of ferrite the reaction of Fe3C to Cr7C3 takes place, and differ-
and different small rod-shaped carbides that distribute ent types of carbide can be found as shown in Fig.
within the ferrite matrix in specific directions (Fig. 18. This has been described previously by Lee [19].
Some investigators [20] found that the Fe3C does not
17). Also, the dislocation cell boundaries and the ran-
transform directly into Cr7C3 but actually dissolves in
dom dislocations situated between these cell
the ferrite matrix whilst the precipitates of Cr7C3
boundaries disappear, whilst a fine cellular structure is
grow elsewhere. In the present study, the Fe3C has a
developed. needle-like structure at low temperature (Fig. 16),
For the case of material tempered at 650°C for 48 whereas Cr7C3 (Fig. 18) is in spheroidal form at the
h, under such a high temperature and such a long high temperature of 650°C. There seems no doubt
time, the AISI 4340 steel has a ferrite matrix with that Fe3C formed both a plate-like appearance and a
carbides scattered throughout it (Fig. 18). After re- spheroidal form to reduce surface energy. From these
crystallisation is complete, growth of carbide particles results it is tentatively concluded that Cr7C3 is proba-
and ferrite grain are the only kinetic processes. At bly formed due to the reaction of Fe3C with the ma-
this tempering temperature, the occurrence of recrys- trix.
Fig. 14. TEM micrograph of a specimen quenched in oil (850°C/30 Fig. 16. TEM micrograph of a specimen quenched in oil (850°C/30
min) and tempered at 200°C for 2 h. min) and tempered at 300°C for 2 h.
206 W.-S. Lee, T.-T. Su / Journal of Materials Processing Technology 87 (1999) 198–206
References