Bull. Mater. Sci., Vol. 34, No. 7, December 2011, pp. 1439–1445. © Indian Academy of Sciences.

Heat treatment and effects of Cr and Ni in low alloy steel

MOHAMMAD ABDUR RAZZAK

Materials and Metallurgical Engineering Department, Bangladesh University of Engineering and Technology
(BUET), Bangladesh

MS received 1 March 2010; revised 14 February 2011

Abstract. The effects of Cr and Ni on low carbon steel was observed. Undissolved carbide particles refine the
austenite grain size. In the presence of nickel, chromium carbide is less effective in austenite grain refinement
than chromium carbide in absence of nickel at temperature below 975°C. Nickel does not produce any austen-
ite grain refinement but presence of nickel promotes the formation of acicular ferrites. It was also found that
Ni and Cr as chromium carbide also refines the ferrite grain size and morphology. Cr as chromium carbide is
more effective in refining ferrite grain size than nickel.

Keywords. Low alloy steel; Cr; Ni.

1. Introduction In the current study four different steels with varying

weight percentages of Ni and Cr were used to observe the
During the last fifty years, there has been a great demand effects of alloying elements. The effects were character-
for steels with higher tensile strength, adequate ductility ized according to the presence of alloying elements either
and toughness. This has been particularly so where light- alone or in conjunction with each other in the low carbon
ness is desirable, as in the automobile and aircraft indus- steel samples. The steel samples were characterized using
tries. An increase in carbon content met this demand in a mechanical testing method. Tensile strength and elonga-
limited way, but even in the heat-treated condition the tion data were collected to compare the effects of heat
maximum strength is about 700 MPa above which value, treatment and alloying elements. Metallographic analysis
a rapid fall in ductility and impact strength occurs and was also done to draw a correlation between alloying
mass effects limit the permissible section (Aver 1974). elements and microstructural feature like grain size and
Heat treated alloy steels provide high strength, high yield morphology.
point, combined with appreciable ductility even in large
sections. The use of plain carbon steels frequently neces-
sitates water quenching accompanied by the danger of 2. Experimental
distortion and cracking, and only thin section can be
hardened throughout. For resisting corrosion and oxida- 2.1 Specimen preparation
tion at elevated temperatures, alloy steels are essential.
The Alloy Steels Research Committee adopted the fol- Four different steels containing about 0⋅11% carbon were
lowing definition: ‘Carbon steels are regarded as steels used in this study. The composition of the steels is pre-
containing not more than 0⋅5% manganese and 0⋅5% sili- sented in table 1. Steel 1 is the base steel with which the
con, all other steels being regarded as alloy steels’ (Ameri- structure and properties of other steels 2–4 are compared.
can Society for Metals 1964). The principal alloying The steels were made previously in an air induction fur-
elements added to steel in widely varying amounts either nace in our department. About 14 mm diameter speci-
singly or in complex mixtures are nickel, chromium, mens were rolled down from 16 mm diameter bars of
manganese, molybdenum, vanadium, niobium, silicon each of the steels in order to study the austenite grain
and cobalt. The observation in this paper is directed to- coarsening behaviour.
wards experiment on low alloy steels (0⋅11 wt% C) which
has a high weldability and toughness. These properties are 2.2 Carburization and measurement of austenite
in high priority for structural steel if these can be blended grain size
in with a high tensile strength. The sole purpose of this
study is to find out proper alloying elements to increase Since size of the austenite grains directly affect the sub-
the tensile properties with appropriate heat treatment. sequent structure and hence the properties of steels, a
study was made to determine prior austenite grain size at
(mohammad.razzak@insa-lyon.fr) temperatures higher than upper critical temperature.
1439
1440 Mohammad Abdur Razzak

Table 1. Composition of the samples.

Composition (wt.%)

Steel no. C Si Mn S P Cr Ni

1 0⋅10 0⋅28 1⋅18 0⋅021 0⋅028 – –

2 0⋅13 0⋅16 1⋅31 0⋅027 0⋅038 – 1⋅26
3 0⋅11 0⋅20 1⋅28 0⋅022 0⋅022 0⋅5 –
4 0⋅11 0⋅20 1⋅28 0⋅022 0⋅022 0⋅69 0⋅97

Carburization technique was used to reveal prior austenite

grain size. There are also other methods in determining
prior austenite grain size like isothermal transformation
technique, oxidation technique, etc. But previous work
showed that the isothermal technique did not work well
in revealing prior austenite grain boundary of low alloy
steels (Haque 1989). So, carburization technique was
adopted to reveal prior austenite grain boundaries of
steels in this work.
The technique is based on the formation of a continu-
ous cementite network at the austenite grain boundaries.
Carbon will diffuse in steel from the carburizing atmos-
phere forming hypereutectoid steel at the surface of the
specimen and during slow cooling in the furnace continu-
ous cementite network is formed at the austenite grain
boundaries at the selected austenitizing temperatures.
Subsequent etching of the furnace cooled samples revealed
the cementite network formed which marked the prior
austenite grain size at the selected carburizing tempera-
tures (Clark and Varney 1962).
Solid carburizing or pack carburizing technique was
applied for this experiment. The steel specimens
were heated to different austenitizing temperatures, i.e.
900–1050°C with an interval of 50°C. Before heating
these specimens, they were packed in a pot with carburiz-
ing mixture. Then they were placed in Blue-M furnace.
After reaching the desired temperature, they were
Figure 1. Variation of prior austenite grain size with tempera-
held at that temperature for 2 h to reach near the equilib- tures for steels 1–4.
rium condition and then cooled in this furnace to
room temperature. Slow cooling ensured a continuous
cementite network through the austenite grain bounda- The heat-treatment temperatures of steels were deter-
ries. mined by a careful examination of the austenite grain
The assessment of prior austenite grain size was made size. The criteria for the determination of the heat-
from direct measurement of the austenite grains in the treatment temperature of steels were that the steel had the
specimens under optical microscope. The grain size was same austenite grain size and that the temperatures were
measured using the mean linear intercept method, count- such that an appreciable proportion of the solute elements
ing grain boundary intersections with the circumference had entered into solution for subsequent precipitation.
of the circle in the eyepiece of a microscope. The effec- This is indicated in figure 1 by a steep rise of the austen-
tive circumference of the circle was determined precisely ite grain size. An austenite grain size of 40 μm was found
by measuring its diameters with reference to a stage to be suitable and the corresponding heat-treatment tem-
micrometer at the magnification used. A total of at least peratures for the steels were 910, 910, 970 and 950°C for
300–600 intersections were counted for each specimen. the steels 1–4, respectively.
Then the size of austenite grain was measured using the Thermodynamic calculation was done using Matcalc
mean linear method. using the database ‘mc_sample’. Calculation of results
 Effects of Cr and Ni in low alloy steel 1441

presented in figure 2 show that chromium in the steels tensile strength (UTS), percentage of elongation (% EL),
precipitated as M3C2. The dissolution temperatures and percentage of reduction in area (% RA).
obtained by the equilibrium thermodynamic calculation is
below the one expected from the experimental one. As
2.4 Optical microscopy of fracture samples
heat treatments were done for 2 h at higher temperatures,
it is logical to expect that the precipitating elements will
Samples from fractured tensile specimens were taken for
be completely in solution at the chosen heat treatment
microscopic examination. To avoid heavily deformed
temperature.
zone for microstructure observation, samples were chosen
from the grip of the tensile test specimen as shown in
2.3 Mechanical testing figure 3. The samples were then ground, polished up to γ-
aluminum powder and then etched in 5% Nital solution.
The heat treated 13 mm diameter bar was then machined The microstructure of these specimens was then studied.
into standard tensile specimens with a nominal diameter Optical microscope photograph (figure 4) of the micro-
and gauge length of 3⋅99 and 25 mm respectively. The structure of each specimen was taken to compare the micro-
grip size was chosen to be 13 mm in width and in length structural features in conjunction with the mechanical
as shown in figure 3. The tensile specimens were properties.
then tested with a Universal Tensile Testing Machine
(INSTRON) to obtain data on yield strength (YS), ultimate
3. Results and discussion

The prior austenite grain size vs temperature graph is

plotted and shown in figure 1. It can be observed from
figure 1 that the austenite grain size increases with in-
creasing austenitizing temperature. For steels 1 and 2 this
relation is almost linear. Steel 1 is a plain carbon steel
and it does not contain any alloying element. So there is
no obstruction for grain growth and the austenite grain
size increases rapidly and linearly with temperature. Steel
2 is basically steel 1 with nickel added to it. This steel
also showed similar austenite grain coarsening behaviour
as that of plain carbon steel 1. Nickel remained in solid
solution and not combined with carbon to produce any
second phase particles. In absence of second phase parti-
cles in steel 2, grain growth is not hindered.
Steel 3 produced the finer austenite grain size than
Figure 2. Matcalc thermodynamic calculation results using steel 1. Cr combines with carbon and forms chromium
mc_sample database for steels 4 and 3. Evolution of phase fraction
is plotted with temperature. carbide precipitates (Aver 1974). These precipitates pin
the austenite grain boundaries and inhibit grain growth
resulting in finer austenite grain size than steel 1 (plain
carbon). Steel 4 also produced grain size finer than steel 1
and coarser than steel 3 (Rollason 1961; Clark and
Varney 1962; Aver 1974). Steel 4 contains both Cr and
Ni. As can be seen from steel 1 nickel does not have any
effect on the austenite grain refinement. So the finer aus-
tenite grain size in steel 4 compared to steel 1 is clearly
due to the effect of chromium carbide precipitates. The
austenite grain size of steel 3 remains finer up to 950°C
beyond this temperature; there is a steep rise in austenite
grain growth. Steel 3 produced finer grain size than steel
4 with (Ni + Cr) up to a temperature of 975°C and above
this temperature steel 4 produced finer austenite grain
size than steel 3. Composition of steel suggested
that steel 3 (Cr = 0.69 wt.%) should contain slightly
Figure 3. Dimensions of tensile specimen used for tensile test higher volume fraction of precipitates than steel 4
and location on sample for subsequent microstructure study is (Cr = 0⋅5 wt.%). Presence of higher volume fraction of
shown. precipitates increased the grain boundary pinning (Zener
1442 Mohammad Abdur Razzak

Figure 4. Optical micrograph showing prior austenite grain boundaries of steels 1–4
revealed by carburization technique at 1000°C (× 200).

pinning) efficiency and thus results in smaller grain size. on the austenite grain size refinement. Finer austenite
The results also indicate that in presence of nickel, chro- grain size of steels 3 and 4 indicated that Cr as chromium
mium carbide is less effective in austenite grain refinement carbide is an effective grain refining element for HSLA.
than chromium carbide in absence of nickel at tempera- The microstructures of steels 1–4 cooled at 120°C/
ture up to 975°C. So, presence of nickel lowers the chro- min are shown in figure 5. It was observed that steels 1–4
mium carbide dissolution temperature in the low alloy showed regular ferrite–pearlite structure with some ferrite
steels. Among the three alloys, steel 2 showed the same morphology change in steel 2. The microstructure
grain coarsening behaviour as plain carbon steel. This observed comprised of fine ferrite–pearlite structure where
confirms the previous understanding that Ni has no effect the pearlite is isolated in the ferritic matrix. Steel 2
 Effects of Cr and Ni in low alloy steel 1443

Figure 5. Optical micrograph of steels 1–4 cooled at 120°C/min (× 200).

at the fast cooling rate of 120°C/min showed some wid- nucleate at relatively low grain mobility condition.
manstatten ferrite along with regular ferrite pearlite. Besides that from the microstructural observation it was
Steels 2–4 produced finer ferrite pearlite than plain car- also clear that Ni modified the ferrite morphology to
bon steel 1. Among the three alloys, steel 3 produced finer more acicular shape.
grain size than steel 2 and steel 4 produced the finest Steel 3 contains Cr. Cr combines with C and formed
grain structure of all steels. Steel 2 has Ni as alloying chromium carbide precipitates during cooling from the
elements; hence it showed smaller grains in comparison austenite zone. These chromium carbide precipitates pin
with the plain carbon steel 1. It is well known that Ni the newly nucleated ferrite grain boundaries and thus fine
lowers the austenite to ferrite transformation temperature ferrite grain is obtained. The finer grain size of steel 3
and thus produced condition for smaller ferritic grains to than steel 2 clearly indicate that Cr as chromium carbide
1444 Mohammad Abdur Razzak

is more effective in ferrite grain size refinement than microstructural observation it is seen that presence of Ni
nickel. Steel 4 contains both Ni and Cr. The finest ferrite promotes acicular ferrite formation. Change in morphology
grain size of this steel is due to the combined effects of of the ferrite to acicular ones also produces obstacle in dis-
nickel and chromium. So it can be said that Cr in pre- location glide. Thus nickel increases the strength by refin-
sence of Ni is more effective in producing finer micro- ing the grains by lowering the transformation temperature
structure. and also changing the morphology of the ferrite grains.
In figure 6, average grain diameter of steels 1–4 is pre- Chromium in the form of chromium carbide precipi-
sented. Grain size measurement also suggested the same tates increased the strength by means of precipitation
phenomenon predicted by microstructural observations. strengthening. Secondary chromium carbides pin the
Considering the experimental error it can be said that grain boundaries and inhibit the grain growth. This
steel 4 (Ni + Cr) has the smallest mean grain diameter of results in grain refinement and presence of second phase
~ 15 μm. Steel 2 showed smaller grain diameter than steel 1 particles also makes dislocation movement more difficult.
but it should be considered that acicular morphology of Second phase particles like chromium carbide in the
ferrite in the microstructure of steel 2 produced greater matrix increases the energy required for elastic/plastic
extent of error in the measurement by mean linear inter- deformation, hence creates higher strength in the alloy.
cept method. So ferrite grain size measurement for steel 2 Percentage of elongation in steels 1, 3 and 4 showed
is not fully reliable. similar results while steel 2 (Ni) with Ni in solid solution
Tensile test results from the specimens of steels 1–4 showed reduced elongation. Microstructural observation
cooled at 120°C/min are shown in figure 7. It is evident showed presence of acicular ferrite in steel 2. Presence of
from the figure that yield strength of steels 2–4 is higher acicular ferrite has the effects of lowering elongation and
than the base steel 1 (PC). Among the three alloy steels, increasing yield strength (Kang et al 2007). In the case of
steel 4 with Ni and Cr produced the highest yield strength steel 4 (Ni + Cr), even with Ni and Cr as alloying ele-
and steel 2 with Ni produced the lowest yield strength. ments did not show change in ferrite morphology, thus
Steel 3 with chromium produced yield strength in the elongation obtained is equal to the base steel 1. It can
between steels 2 and 4. A similar trend was found with be expected that the presence of second phase particles
the ultimate tensile strength of these steels. The higher and smaller grain size in steels 3 and 4 should yield less
yield strength of steel 3 with Cr than steel 2 with Ni indi- elongation which is contradictory with the experimental
cated that Cr is more effective than nickel in increasing results obtained. The explanation can be given from the
yield strength. The highest yield strength of steel 4 with point of view of the fraction of pearlite present in the
Ni and Cr is clearly due to the combined effects of Ni and microstructure and its distribution. Presence of second
Cr. phase particle decreased the amount of carbon available
Nickel does not produce any second phase particle. Ni in the matrix. Smaller weight fraction of carbon available
is found mostly in the form of solid solution in the ferrite during cooling should yield lower fraction of pearlite in
(Rollason 1961; Clark and Varney 1962; Aver 1974). the microstructure in comparison with the base plain car-
So Ni increased the strength of the steel by solid solution bon steels 1 and 2 (Ni). Lower volume fraction of pearlite
strengthening. Besides that Ni also lowers the transforma- in the microstructure in conjunction with finer distribu-
tion temperature (Rollason 1961; Clark and Varney tion increased the deformability in steels 3 and 4. The
1962; Aver 1974), so the lower transformation tempera- effects of second phase particles and smaller ferrite
ture produces smaller ferrite grains. Besides that from the grains in decreasing ductility is somewhat countered by
the effects of change in distribution and lower fraction of
pearlite in the microstructure in increasing ductility.

Figure 7. Comparison of yield strength and elongation of

Figure 6. Average grain diameter of steels 1–4. steels 1–4 cooled at 120°C/min.
 Effects of Cr and Ni in low alloy steel 1445

4. Conclusions to increase yield strength is more than that of chromium

carbide in the absence of nickel.
The carburization technique is a reasonably satisfactory
method in revealing the prior austenite grain boundaries
in low carbon steels containing nickel and chromium. On References
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refined the austenite grain size. In the presence of nickel, Park, Ohio: American Society for Metals) 8th edn, Vol. 2
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refinement than chromium carbide in absence of nickel at McGraw-Hill Book Company) 2nd edn
temperature below 975°C and the reverse is true above Clark D S and Varney W R 1962 Physical metallurgy for
975°C. Nickel did not produce any austenite grain engineers (New York: Litton Educational Publishing Inc.)
refinement. Nickel and chromium as chromium carbide 2nd edn
precipitates were found to refine the ferrite grain size. Cr Haque Mohammad Zahirul 1989 Effect of alloying elements in
is found to be more effective in the refinement of ferrite HSLA, MSc Engg. Thesis, Department of Metallurgical Engi-
neering, BUET, Dhaka, pp 130–150
grain size than nickel. Nickel in solution and chromium
Kang J S, Huang Y, Lee C W and Park C G 2007 Adv. Mater.
as chromium carbide precipitates increased the yield Res. 15–17 786
strength of the low carbon steels but the effectivity of Rollason E C Metallurgy for engineers (London: Edward
chromium carbide precipitates in the increment of yield Arnold Publisher) 3rd edn
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presence of nickel the contribution of chromium carbide carbides in a Fe–Cr–C alloy