Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

doi:10.4236/jcpt.2013.34025

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Journal of Crystallization Process and Technology, 2013, 3, 163-169

http://dx.doi.org/10.4236/jcpt.2013.34025 Published Online October 2013 (http://www.scirp.org/journal/jcpt)

163

Recrystallization Kin etics and Microstructure Evolution of

Annealed Cold-Drawn Low-Carbon Steel

Nurudeen A. Raji, Oluleke O. Oluwole

Department of Mechanical Engineering, University of Ibadan, Ibadan, Nigeria.

Email: [email protected], [email protected]

Received July 23rd, 2013; revised August 23rd, 2013; accepted August 30th, 2013

Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is

properly cited.

ABSTRACT

The recrystallization behavior of cold-drawn 0.12 wt% C steel during annealing at temperatures 600˚C and 650˚C was

investigated. Hardness tests were used to characterize the recrystallization kinetics. The micrographs of the steel were

obtained using optical microscopy (OM) to characterize the grain microstructure of the non-treated and the annealed

steel samples. Annihilation of dislocation defects occur within the soaking time of 5 - 10 minutes for all the deformed

steel after annealing at 650˚C. Specifically at 5 minutes soaking time the grains elongation is still observed indicating

that reformation of grains is not taking place but recovery of the deformed grains. At the 10 minutes annealing time,

new grains are observed to begin and full recrystallization is achieved at 15 minutes annealing time. At annealing time

between 20 - 25 minutes, grains coarsening are observed indicating the onset of grain growth. The hardness of the ma-

terial reduces with increasing annealing temperature for all the degree of cold drawn deformation. On the basis of the

experimentally obtained hardness values, recrystallization increases with increasing degree of cold drawn deformation

for the annealed steel. Recovery process was found to prolong in the 20% cold drawn steel as compared to the 55% cold

drawn steel. The prolong recovery process is due to reduction in the driving force. Full recrystallization of the annealed

steel is achieved at different soaking time depending on the degree of the cold drawn steel.

Keywords: Drawn Steel; Recovery; Recrystallization; Microstructure; Hardness; Soaking Time

1. Introduction

Drawn steel is products of metal drawing process which

include bar or rod drawing, tube drawing and wire draw-

ing. This drawing process has been widely used to ma-

nufacture fine wires, tension loaded structural compo-

nents, springs, paper clips, spokes for wheels and plain

nails [1,2]. The wire drawing process reduces the cross-

section of a wire by pulling it through series of drawing

dies of decreasing diameter to produce wires of desired

diameters. It is mostly performed at room temperature

and thus is classified as cold-work process. The original

metal usually consists of strain-free crystal grains [3].

When the metal is deformed by cold drawing, dislocation

and other imperfections such as vacancies are introduced

into the crystal structure generating microstructure het-

erogeneities that exhibit large orientation gradient [4].

The grains then acquire a preferred orientation or texture.

The structural changes which occur include the gradual

stretching of the grains in the direction of principal de-

formation and accumulation of dislocation and some

other defects [5]. The accumulation and migration of the

dislocation due to the cold drawing process results in

strain hardening of the steel allowing for increase in its

tensile strength with reduced ductility [6]. The degree of

cold-drawn deformation determines whether the steel

will attain a brittle nature or remains ductile [7]. The

strain hardening also known as work hardening is an in-

crement in internal energy associated with an increase in

the dislocation density as well as density in point defects,

such as vacancies and interstitials [8,9]. Some other ef-

fects of such cold work on the properties of polycrystal-

line structures have been studied extensively [10-20].

The individual grain of a polycrystalline material chang-

es relative to the direction of applied stress during the

deformation which is distributed heterogeneously among

the individual grains [21]. A typical feature of such de-

formed structure is anisotropy of mechanical properties.

An initially isotropic material responds by developing

anisotropy when subjected to inelastic deformation. The

Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

164

inelastic induced anisotropy includes directional anisot-

ropy in cold worked metals [22]. These changes in the

mechanical properties of the steel due to the deformation

often influence the performance of the resulting product

of the process in service. In the case of wire drawing pro-

cess for plain nail manufacture, the steel is cold-drawn to

sizes at 20%, 25%, 40%, and 55% for the manufacture of

4 inches, 3 inches, 2.5 inches and 2 inches respectively.

During the drawing operation the carbon steel experi-

ences microstructure changes which affect the mechani-

cal properties of the steel and consequently the perform-

ance of the resulting product in service [23]. The associ-

ated problems include high strain hardening of the steel

due to the degree of plastic deformation which causes

nail brittleness or poor ductility resulting in buckling of

the nail in service. The large amount of internal strain in

the form dislocation as a result of the strain hardening

means that energy is stored in the metal. This energy can

be released through heat treatment, where energy in the

form of heat is introduced into the material allowing the

release of stored energy in the process of recrystallization

[24]. Recrystallization is the reconstruction of the grain

structure during annealing of deformed metals. It causes

a change in the grain structure of the material that has

been previously cold-worked or plastically deformed.

The recrystallization process tends to eliminate the dis-

locations by means of migration of high-angle grain

boundaries driven by the stored energy of deformation

and a new grain structure in the deformed material

evolved. [25,26]. Thus, new dislocation-free grains are

formed within the recovered structure. The new grains

then grow at the expense of the old deformed grains,

leaving a new structure with low dislocation. The new

structure consumes the old grains, resulting in a new

grain structure with a very or no low dislocation density

[27].

Recrystallization is a function of the amount of strain

induced during deformation as well as the time and tem-

perature of annealing [28]. In this study, the recrystalli-

zation kinetics and the corresponding microstructure evo-

lution in annealed cold-drawn low carbon steel is inves-

tigated according to annealing time by mechanical test

and microstructure characterization. The kinetics of re-

crystallization involves determining the fraction of re-

crystallized grains with annealing time which is used to

describe the evolution of the recrystallized grains with

increasing time of annealing at a particular temperature

[29]. The studies of the recrystallization kinetics have

shown that the mechanical properties of metallic materi-

als could be controlled by the microstructure of the mate-

rial [28,30,31]. The control of the microstructure of the

steel could therefore be used to obtain desired mechanic-

cal properties for the steel. The idea of control of me-

chanical properties in materials through these processing

techniques has been studied [32].

Recrystallization is a thermally activated process, con-

sisting of the generation of strain-free grains and their

growth at the expense of the deformed grains until the

deform grain is entirely consumed [28]. And the driving

force for recrystallization is the energy stored in the ma-

terial during deformation [33]. The purpose of recrystal-

lization is to refine the grains for improved properties

and important mechanical properties can be restored after

annealing of cold deformed steel allowing for further de-

formation.

The generally accepted empirical model used to de-

scribe recrystallization kinetics is the Johnson-Mehl-Avra-

mi-Kolmogorov (JMAK) expressed [28,30,33] as:

1exp n



 



where v

the volume recrystallized, k is the JMAK

variable which is temperature dependent and n is the

JMAK exponent and t is the annealing time.

The model was developed on the assumption that the

recrystallized nuclei form randomly in the cold-worked

microstructure and that the growth of the nuclei is iso-

tropic but real materials do not exhibit this behavior be-

cause of the non-uniform distribution of the stored en-

ergy, non-random distribution of the nuclei and anisot-

ropic growth of recrystallized nuclei [34]. It is therefore

of importance to consider real situation of the recrystal-

lization process through experimentation as input for a

realistic model.

This paper considered the use of the micro hardness

property of the annealed cold drawn low carbon steel at

different temperature and soaking time to investigate the

recrystallization process for desired mechanical proper-

ties.

2. Materials and Methods

The low carbon steel used for this study is obtained from

Nigeria Wire Industry Ltd, Ikeja, Nigeria. The average

chemical composition for the steel is as given in Table 1.

Samples of wire cold-drawn by 25% and 40% degree of

deformation were obtained. A Muffle furnace, Gallen-

komp® model SVL-1009 with voltage regulation of 220

V, 50 Hz of temperature range 300˚C ~ 1000˚C obtained

in the materials test laboratory of Igbinedion University,

Okada was used to annealed the steel at 650˚C and

700˚C for time interval ranging from 5 minutes to 60

minutes.

Table 1. Chemical composition of the as-received steel wire

material (wt%).

C Si Mn P Fe

0.12 0.18 0.14 0.7 98.86

Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

165

The samples for evaluation of the microstructures by

optical microscopy (OM) were cut from the annealed

wire, and taken through a grinding process on silicon

carbide paper, 240, 320, 400, and 600 grit. The samples

were then polished initially at 1μm and finally at 0.5 μm

using emery cloth and silicon carbide solution, etched

with 2% nital and the metallography was carried out us-

ing the optical microscope (OM) with image capturing

device. The hardness test was done on a Brinnel tester. In

preparation for hardness measurements, scaling on the

surface of each of the annealed specimens was removed

in the area where the test was to be conducted. A wire

brush was used to remove the surface scaling. Each speci-

men for the hardness test was filed to create flat surface

on the nail shank. The flat surface was then polished with

emery paper to obtain very smooth surface required of

the test. The Brinnell test for this experiment employed a

1-mm diameter carbide ball which was pressed onto the

specimen by a 1750-g load that was maintained for 10

seconds. The diameter of the indenter impression was

measured with the Brinnel reading microscope of magni-

fication 20× and the measurement converted to the Bri-

nell-Hardness Number on the Brinnel tester conversion

table.

The recrystallization fraction is determined based on

the hardness measurement using Expression (1) [33].



initial

initial final

BHNBHN t

BHN BHN

X

 (1)

where initial

BHN the hardness of the deformed sample,

final

BHN is the hardness of the fully recrystallized sam-

ple and



BHN t is the hardness after a given soaking

time.

3. Results and Discussion

3.1. Microstructure Evolution

Figures 1(a)-(f) show the microstructure evolution of the

25% cold-drawn low-carbon steel and as annealed at

650˚C for annealing time range of 5 - 20 minutes. The

microstructure of the cold-drawn steel shown in Figure

1(a) non-treated is inhomogeneous with accumulating

dislocation density concentrated at the grain boundaries

as indicated by the large area of dark patterns of the

structure. After annealing the drawn steel at 650˚C for a

soaking time of 5 - 10 minutes, annihilation of the dislo-

cation is observed with most of the dark patterns clearing

off the structure. Specifically at 5 minutes soaking time

as shown in Figure 1(b), the grains elongation is still

observed indicating that reformation of grains is not tak-

ing place but recovery of the deformed grains which in-

volves movement of low-angle grain boundaries. At the

10 minutes annealing time, new grains are observed to

begin to form as shown in Figure 1(c) and full recrystal-

lization is achieved at 15 minutes annealing time as

shown in Figure 1(d). At annealing time between 20 - 25

minutes, grains coarsening are observed indicating the

onset of grain growth. This is usually avoided in-order to

keep the required strength of the material.

3.2. Material Hardness

Figures 2-5 show the steel hardness measured from the

Brinnel hardness test as a function of the soaking time at

different annealing temperature for the 20%, 25%, 40%

and 55% cold drawn steel respectively. It is observed that

recrystallization could be said to start after 600 seconds

at all the applied annealing temperatures. The hardness of

(a) (b) (c)

(d) (e) (f)

Figure 1. (a) As-received cold-drawn at 25%; (b) annealing time of 5 min; (c) annealing time of 10 min; (d) annealing time of

15 min; (e) annealing time of 20 min; (f) annealing time of 25 min.

Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

166

190

195

200

205

210

215

220

225

230

235

01000 2000 3000 4000

BHN

Soakingtime(sec.)

Annealed20%col ddrawn

500deg.C

550deg.C

600deg.C

650deg.C

700deg.C

Figure 2. Influence of soaking time on hardness of annealed 20% cold drawn 0.12 wt% C steel.

180

200

220

240

260

280

300

01000 2000 3000 4000

BHN

Soakingtime(sec.)

Annealed25%colddrawn

500de g.C

550de g.C

600de g.C

650de g.C

700de g.C

Figure 3. Influence of soaking time on hardness of annealed 25% cold drawn 0.12 wt% C steel.

200

220

240

260

280

300

320

340

01000 2000 3000 4000

BHN

Soakingtime9sec.)

Annealed40%colddrawn

500deg.C

550deg.C

600deg.C

650deg.C

700deg.C

Figure 4. Influence of soaking time on hardness of annealed 40% cold drawn 0.12 wt% C steel.

200

220

240

260

280

300

320

340

360

01000 2000 3000 4000

BHN

Soakingtime(sec. )

Annealed55% col d drawn

500deg.C

550deg.C

600deg.C

650deg.C

700deg.C

Figure 5. Influence of soaking time on hardness of annealed 55% cold drawn 0.12 wt% C steel.

Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

167

the material reduces with increasing annealing tempera-

ture for all the degree of cold deformation. This implies

that rate of recrystallization increases with increasing

annealing temperature.

3.3. Recrystallization Kinetics

The evolution of the recrystallization was measured by

the Brinnel hardness during the annealing at 600˚C and

650˚C. Table 2 shows the hardness values of the steel.

The maximum and minimum hardness values were

measured from the hardness test such that the maximum

hardness correspond to the hardness of the material at

time of zero seconds which is the hardness of the de-

formed material without annealing and the minimum

hardness correspond to the hardness of the fully recrys-

tallized grain.

The relationship between the recrystallization kinetics

and soaking time showing the influence of the degree of

cold drawn deformation are shown in Figures 6 and 7 for

the 20%, 25%, 40% and 55% degree of cold drawing

annealed at temperatures of 600˚C and 650˚C. The fig-

ures show truncated sigmoidal shape lacking the small

slope region which usually describe the nucleation period

of recrystallization. This could be explain that the lack of

the clear nucleation region of the curves is as a result of

prolonging recovery process which tends to reduce the

driving force required for nucleation at lower soaking

time. The extent of recovery decreases with increasing

degree of cold drawn deformation. The prolonged recov-

ery process in the 20% and 25% cold drawn steel could

be as a result of reduction in the driving force required

for nucleation at lower soaking time. It is also observed

that the rate of recrystallization increases with increasing

degree of cold drawn deformation. This means that re-

covery process is faster in the highly cold drawn steel.

The influence of recovery is to cause the recrystallizing

grain growth rate to decrease continuously during recrys-

tallization. The figures show that full recrystallization of

the grains commenced at different soaking time for the

cold drawn steel depending on the degree of cold drawn

deformation.

4. Conclusion

The microstructure evolution of cold drawn 0.12 wt% C

steel has been analyzed. The accumulated dislocation due

to cold drawing deformation of the steel annihilate after

annealing the drawn steel at 650˚C for a soaking time of

5 - 10 minutes, annihilation of the dislocation is observed

with most of the dark patterns clearing off the structure.

At lower soaking time, recovery of the deformed grains

is pronounced. Recrystallization of the grains com-

menced after annealing for soaking time of 10 minutes.

At annealing time between 20 - 25 minutes, grains coars-

ening are observed indicating the onset of grain growth.

The hardness of the material reduces with increasing

annealing temperature for all the degree of cold deforma-

tion indicating increasing recrystallization with increase-

ing annealing temperature. The kinetics of recrystalliza-

tion has been described with the hardness test values for

cold drawn 0.12 wt% C steel annealed at 600˚C and

Table 2. Initial and recrystallized values for hardness of

cold drawn 0.12 wt% C steel.

Deformation BHNinitial

BHNfinal

(annealed at 600˚C)

BHNfinal

(annealed at 650˚C)

20 230 201.2 197.91

25 281.65248.3 221

40 315.67257.7 234.6

55 336 296 248

0.7

0.75

0.8

0.85

0.9

0.95

1.05

01000 2000 3000 4000

Fr actionr ecrystallized

soakingtime,sec.

20%colddrawn

25%colddrawn

40%colddrawn

55%colddrawn

Figure 6. Recrystallization kinetics of cold drawn 0.12 wt% C steel annealed at 600 deg. C.

Recrystallization Kinetics and Microstructure Evolution of Annealed Cold-Drawn Low-Carbon Steel

168

0.7

0.75

0.8

0.85

0.9

0.95

1.05

01000 2000 3000 4000

Fractionr ecrystallized

soakingtime,sec.

20%colddrawn

25%colddrawn

40%colddrawn

55%colddrawn

Figure 7. Recrystallization kinetics of cold drawn 0.12 wt% C steel annealed at 650 deg. C.

650˚C. The recrystallization kinetic is characterized by

prolonged recovery at lower soaking time and rate of

recrystallization increases with increasing degree of cold

drawn deformation. Full recrystallization is achieved faster

in the highly deformed steel.

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