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AISTech 2019 — Proceedings of the Iron & Steel Technology Conference

6–9 May 2019, Pittsburgh, Pa., USA


DOI 10.1000.377.205

Study On Removal Of Brittle Phases By Optimizing The Process Parameters Of Welding Wire
Rod Grade For Gas-Metal Arc Welding Applications

E.Sakallı1, S.Günbay2, H.Gül3, A.Sağlam2, D.Özyiğit1, E.Gönülalan3, O.Gündüz1

1 ERDEMIR, R&D
Uzunkum Cad. No:7, P.O. Box 67330,
Kdz.Ereğli, Zonguldak,Turkey
Phone: +903723298709
Email: esakalli@erdemir.com.tr, dcimen@erdemir.com.tr, ogunduz@erdemir.com.tr

2 ISDEMIR, Quality Metallurgy


Karayılan, Payas, P.O. Box 31319,
Iskenderun, Hatay, Turkey
Email: sgunbay@isdemir.com.tr, ahsaglam@isdemir.com.tr

3 ISDEMIR, Wire Rod Mill


Karayılan, Payas, P.O. Box 31319,
Iskenderun, Hatay, Turkey
Email: hgul@isdemir.com.tr, egonulalan@isdemir.com.tr

Keywords: Gleeble 3500, JMatPro, martensite, CCT, SEM, welding wire

INTRODUCTION
Welding wire rod grade has a wide range of applications like fame fabrication, automotive structures, farm implements,
construction equipment, pressure vessels, pipe fabrication, railcar construction and repair, general fabrication and it is also
widely used in high-speed robotic and automatic welding applications and semi-automatic applications [1]. The objective of
this study was to prevent breakages and improve drawability in customer lines especially in wet wire drawing process from
2.0 mm to 1.2, 1.0 and 0.8 mm.
Main customer requirements from this grade were good drawability during wire drawing process from 5.5 mm diameter wire
rod in coils down to 0.8 mm, no breakage, ferritic- perlitic microstructure not including brittle phases as in Figure 1, good
surface quality, tensile strength less than 570 MPa, RA(%) not less than 78. So this study is based on optimizing chemical
composition and process parameters of this welding wire rod grade for gas metal arc welding application to ensure the
customer requirements. Early trials failed especially in wet wire drawing process from 2.0 mm to 1.2, 1.0 and 0.8 mm. due to
breakage Typical chemical composition and mechanical properties for this grade of the previous trials were given in Table 1.

Table 1. Chemical composition and mechanical properties.

Chemical Composition (% ) Mechanical Properties


C Mn Si Tensile Strength (Max.) Reduction in Area (Min.)
Typical Range 0.060- 0.090 1.60-1.75 0.85-0.95 570 MPa 78%
Previous Trials 0.075- 0.090 1.70-1.75 0.90-0.95 570 MPa 78%

In this study, experimental techniques such as physical simulation, microscopy and micro chemical analysis were used
together with computational materials engineering software to identify the root cause and resolve the quality issues
accordingly. Investigations showed that breakage is associated with the presence of brittle phases, center star

© 2019 by the Association for Iron & Steel Technology. 1987


cracks/segregation, inclusions, insufficient homogeneous slow cooling in Stelmor® line, chemical composition in upper
limits, nonhomogeneous cooling in cooling box. After optimizing the chemical composition and process parameters in both
steelmaking, continuous casting and rolling mill side main customer requirements were provided and this grade was
produced successfully in customer lines without breakage by satisfying the customer demands. This paper includes mainly
rolling mill side optimizations. Also improvements were done in steelmaking, continuous casting sides like optimizing super
heat, cooling in mould sections, EMS (electromagnetic stirring) and more to prevent center star cracks/segregation and
detrimental inclusions (Figure 2).

X500 – Nital (2%) X500 – LePera Hardness vs. C (wt%) Diagram [2]

163 HV 0.02 kg 265 HV 0.02 kg 784 HV 0.02 kg (brittle phase)

Figure 1. Comparison of Nital & LePera etchants for phases martensite & pearlite and hardness values of matrix and brittle
phases. M; martensite, P;Pearlite

1988 © 2019 by the Association for Iron & Steel Technology.


X25 X100 X500

Si Ca Sum Spectrum

O
Mg
Mn
Al

C S Ca
Ca S Mn Mn

0 1 2 3 4 5 6 7 8 9 10
Full Scale 1012 cts Cursor: -0.087 (0 cts) keV

Figure 2. SEM –EDS center star cracks/segregation and inclusion analysis.

EXPERIMENTAL PROCEDURE
Chemical compositions in this study were specifically chosen according to DIN 8559-P1 SG3 (1984) standard, due to
previous experiences and customer requirements to produce wire rod for welding wire applications. As rolled samples were
prepared with these compositions to determine CCT (Continuous Cooling Transformation) diagrams and to perform
Stelmor® line thermal cycles using Gleeble 3500 thermo-mechanical physical simulator to understand the material behavior
during different process conditions. Also JMatPro® software was used to verify the Gleeble 3500 thermal simulator results.
Gleeble 3500 thermal simulator and the samples for CCT and Stelmor® line cooling simulations are provided in Figure 3.

© 2019 by the Association for Iron & Steel Technology. 1989


(a) Samples for Stelmor® line cooling simulation

(b) Samples for CCT


Figure 3. Gleeble 3500 thermal simulator and samples (a),(b) prepared for Gleeble.
In previous trials chemical compositions were in upper limits of the typical range as given in Table1. After sample
preparation, first cooling patterns of previous trials were applied to Gleeble 3500 simulator by using samples which were in
upper limits of the typical range of chemical composition to understand the microstructure. Next chemical composition was
revised to lower limits and CCT curves were derived experimentally using Gleeble 3500 simulator`s dilatometer and
computationally using JMatPro® software. Then, some cooling patterns were determined by using CCT curves obtained from
Gleeble 3500 and JMatPro® software to obtain ferritic-pearlitic martensite free microstructure to fulfill the customer
requirements. Furthermore, the determined patterns were simulated by Gleeble 3500 and JMatPro® software. Possible phases
among these determined cooling patterns were described by using JMatPro® software. Then, the same thermal cycles were
applied to Gleeble 3500 simulator to verify the microstructure that we obtained from JMatPro® software. For simulating the
Stelmor® line thermal cycles by Gleeble 3500 thermal simulator, sample shown in Figure 3 was used. During analyzing
microstructure Hardness test, SEM, SEM-EBSD analyses were done also to describe the brittle phases.
Finally industrial trials were done throughout the optimum process conditions and the same chemical compositions that were
determined after experimental studies. Figure 4 shows the wire rod mill where the industrial trails were done after
experimental studies were completed. Length of Stelmor® line in this mill is 67mt. It has ~48 mt covered section on
Stelmor® line after laying head. One of the main restriction in this study was the length of the Stelmor® line covered section.
During this study in this rolling mill, the 130 mm square billets were rolled to 5.5 mm diameter wire rod in coils.

1990 © 2019 by the Association for Iron & Steel Technology.


67 meters

Figure 4. Layout of the rolling mill for industrial trials [3]


During the industrial trials, results of previous trials which had chemical composition in upper limits including center star
cracks/segregation, detrimental inclusions and insufficient slow cooling in Stelmor® line compared with trials which has
revised chemical composition in lower limits of the typical range, not including center star cracks/segregation, detrimental
inclusions and also has optimum slow cooling in Stelmor® line according to mechanical properties, microstructure analysis
by using optical microscope, hardness tests, SEM, SEM EBSD analyses and also drawability in customer line was
investigated.

RESULTS AND DISCUSSION


Chemical compositions of trials are given in Table 2. Studies have been done according to these chemical compositions. Trial
1 is the typical chemical composition of previous trials and Trial 2 is the revised chemical composition according to previous
investigation results. Firstly, CCT and TTT diagrams were simulated by using JMatPro® software.

Table 2. Chemical compositions of trials.

Composition [ wt % ] C Mn Si
Trial 1 0.085 1.72 0.93
Trial 2 0.068 1.60 0.86

TTT and CCT diagrams were calculated using JMatPro® software for an austenitization temperature of 900°C and a prior
austenite grain size ASTM 9 are presented in Figure 5.

© 2019 by the Association for Iron & Steel Technology. 1991


Pearlite 1%
Pearlite 1%

Figure 5. Calculated TTT and CCT diagrams of analysis in Trial1 (Previous Trial) (Taust = 900°C, ASTM 9)
Moreover, Gleeble 3500 simulator has been used to validate CCT diagrams determined by JMatPro® software. As-rolled
samples prepared as shown in Figure 3 were used to simulate CCT diagrams in Gleeble 3500. Figure 7 illustrates the
experimentally determined CCT diagram. Comparison of Figure 6 and 7 indicates a fairly good agreement between
calculations and experiments. Thus, the software was considered as a validated tool for further improvement of the process.

Pearlite 1% Pearlite 1%

Figure 6. Calculated TTT and CCT diagrams of new analysis in Trial2 (New Trial) (Taust = 900°C, ASTM 9)

Figure 7. Experimentally determined CCT diagram.


Secondly, Stelmor® line cooling process simulations, which are presented in Table 3, have been determined considering the
computational and experimental data derived in the previous step. Simulated Stelmor® line cooling patterns were shown in
Table 3. Then to describe the possible phases which could be formed by using the cooling patterns were determined using
numerical simulation. After that physical simulation of the process was used to validate the determined cooling patterns for

1992 © 2019 by the Association for Iron & Steel Technology.


microstructural studies. In general again, a good agreement was found between the numerical and physical simulations. Main
difference in these cooling patterns are laying head temperature and cooling rate under covered section on Stelmor® line.
In previous trials main problem was poor insulation under covered section on Stelmor® line which result in heat loss.
Cooling patterns 1-4 in Table 3 are the patterns of the previous trials which were applied before the improvements on
Stelmor® line. To achieve the cooling rates in patterns 5-8 in Table 3 some improvements have been done under covered
area on Stelmor® line for insulation. In order to obtain adequate homogeneous slow cooling steel sheets were added under
conveyor, 3 more covers in 4th section of the conveyor line and improved covers positioning. Microstructure results related
with the cooling patterns were shown in Figures 8. During micro examinations in some cooling patterns, especially with high
laying head temperatures, chemical composition in upper limits as in Trial1 including center star cracks/segregation,
detrimental inclusions and has inadequate homogeneous slow cooling in Stelmor® line, brittle phases were detected as in the
previous trials.

Table 3. Stelmor® line Cooling Patterns for Trial1 & Trial2.


Covered  Covered 
Cooling Rate  Cooling Rate  Reforming  Cooling Rate After 
Austenitization  Laying Head  Section  Section 
Trial No Cooling Pattern Under Covered  After Covered  Station Temp.  Reforming Station 
Temp. (°C) Temp. (°C) Start Temp.  Exit Temp. 
Section (°C/sec) Section (°C/sec) (°C) Temp. (°C/sec)
(°C) (°C)
Trial 1 1 900 860 820 0.264 600 0.67 500 ≤ 1
Trial 1 2 900 820 780 0.264 560 0.67 460 ≤ 1
Trial 1 3 900 800 760 0.264 540 0.67 440 ≤ 1
Trial 1 4 900 780 740 0.264 520 0.67 420 ≤ 1
Trial 1 5 900 860 820 0.18 640 1.14 540 ≤ 1
Trial 1 6 900 820 780 0.18 600 1.14 520 ≤ 1
Trial 1 7 900 800 760 0.18 580 1.14 500 ≤ 1
Trial 1 8 900 780 740 0.18 560 1.14 480 ≤ 1

Covered  Covered 
Cooling Rate  Cooling Rate  Reforming  Cooling Rate After 
Austenitization  Laying Head  Section  Section 
Trial No Cooling Pattern Under Covered  After Covered  Station Temp.  Reforming Station 
Temp. (°C) Temp. (°C) Start Temp.  Exit Temp. 
Section (°C/sec) Section (°C/sec) (°C) Temp. (°C/sec)
(°C) (°C)
Trial 2 1 900 860 820 0.264 600 0.67 500 ≤ 1
Trial 2 2 900 820 780 0.264 560 0.67 460 ≤ 1
Trial 2 3 900 800 760 0.264 540 0.67 440 ≤ 1
Trial 2 4 900 780 740 0.264 520 0.67 420 ≤ 1
Trial 2 5 900 860 820 0.18 640 1.14 540 ≤ 1
Trial 2 6 900 820 780 0.18 600 1.14 520 ≤ 1
Trial 2 7 900 800 760 0.18 580 1.14 500 ≤ 1
Trial 2 8 900 780 740 0.18 560 1.14 480 ≤ 1

© 2019 by the Association for Iron & Steel Technology. 1993


Possible phases obtained by Cooling Pattern 1 -Trial1 Cooling Pattern 1 Trial1
JMatPro® Software X500 – Nital (2%) X500 – LePera

M
Pearlite

Possible phases obtained by Cooling Pattern 5 -Trial1 Cooling Pattern 5 Trial1


JMatPro® Software X500 – Nital (2%) X500 – LePera

Pearlite
M

Figure 8.Possible phases obtained by JMatPro® Software. Microstructure of some cooling patterns M; martensite
In pattern 2-3 especially with chemical composition in Trial 2 relatively better results were obtained when compared to Trial1
pattern 1-5. But brittle phases were not totally disappeared in those patterns. Size of them are around less than 12 microns
with less frequency. According to previous investigations and experimental studies to eliminate the brittle phases best
patterns were 6-7 with chemical composition of Trial2. Composition of Trial1 was also experienced with these patterns but it
was not succeeded to remove brittle phases completely because of higher C-Mn content. The results were shown in Figure 9.
In patterns with laying head temperature 780°C also good results were obtained in microstructure. However, because of the
temperature range while cooling from mono block to laying head, acicular ferrite and inhomogeneous structure (Figure 10)
occurs on the surface of wire which causes breakages in customer line.

1994 © 2019 by the Association for Iron & Steel Technology.


Possible phases obtained by Cooling Pattern 6 –Trial2 Cooling Pattern 6 Trial2
JMatPro® Software X500 – Nital (2%) X500 – LePera

Pearlite

Possible phases obtained by Cooling Pattern 7 –Trial2 Cooling Pattern 7 Trial2


JMatPro® Software X500 – Nital (2%) X500 – LePera

Pearlite

Figure 9. Possible phases obtained by JMatPro® software. Microstructure of some cooling patterns

X100 X200 X500

213 HV0.05

192 HV0.05

159 HV0.05

162 HV0.05

Figure 10. Inhomogeneous microstructure.


Finally, for industrial trials Trial2 chemical composition and optimum values of cooling patterns 6-7 were used. Also some
improvements were done in steelmaking, continuous casting sides like optimizing super heat, cooling in mould sections,
EMS (electromagnetic stirring) and etc. to prevent center star cracks/segregation and detrimental inclusions. The results of
the newly produced 5.5 mm diameter wire rod with optimum process conditions and drawn wires to 0.8 mm in customer lines
were compared with the previous failed process final products before improvements on Stelmor® line with Trial1’s chemical
composition which was in upper limits of the typical range of this grade. Comparison of new industrial trials and previous
failed trials were shown in Figure11 by means of microstructure obtained from optical microscope for 5.5 mm diameter wire

© 2019 by the Association for Iron & Steel Technology. 1995


rod samples. For detailed investigation of phases besides optical microscope Jeol JSM 7100F FEG-SEM was used. SEM
investigations showed that new trials were consist of fully ferritic-pearlitic microstructure, while previous failed ones were
including brittle phases as shown in Figure 12.

New Trials- Trial2 ChemicaL Composition & Optimized Cooling Pattern 6-7 Microstructure
X25 X500 – Nital (2%) – Center X500 – LePera - Center

Previous Trials- Trial1 Chemical Composition & Early Trials Cooling Patterns 1-4 Microstructure
X25 X500 – Nital (2%) - Center X500 – LePera - Center

Previous Trials- Trial1 Chemical Composition & Early Trials Cooling Patterns 1-4 Microstructure
X25 X500 – Nital (2%) - Center X500 – LePera - Center

Figure 11. Comparison of microstructure of New Industrial Trials and Previous Failed Trials

1996 © 2019 by the Association for Iron & Steel Technology.


Previous Trials- Trial1 Chemical Composition & Early Trials Cooling Patterns 1-4 Microstructure
X2500 X5000

F
M
M
P

New Trials- Trial2 Chemical Composition & Optimized Cooling Pattern 6-7 Microstructure
X1500 X2500

Figure 12. Comparison of microstructure of New Industrial Trials and Previous Failed Trials (SEM , M; Martensite, F;
ferrite, P; pearlite.
In addition to these 0.8 mm drawn wires were investigated in customer lines. Previous failed ones were compared with new
trial. Breakages were noticed in customer line while wet drawing process from 2.00 mm to 0.8 mm in previous trials.
However in new trials good drawability were obtained without breakage in wet drawing process from 2.00 mm to 0.8 mm.
For comparison of trials drawn wires were investigated by optical microscope and Jeol JSM 7100F FEG-SEM (Figure13-14).
Identification and quantification of the brittle phases were investigated with EBSD method. In order to do this, Nordlys Nano
EBSD detector that is attached to Jeol JSM 7100F FEG-SEM instrument was used. (Figure 15).

© 2019 by the Association for Iron & Steel Technology. 1997


Previous Trials- Trial1 Chemical Composition & Early Trials Cooling Patterns 1-4 Microstructure

X25-Polished X500 – Nital (2%) X3000 – SEM

Figure 13. Microstructure of wet drawn wire in Previous Failed Trials (Breakage).

New Trials- Trial2 ChemicaL Composition & Optimized Cooling Pattern 6-7 Microstructure
X25-Polished X500 – Nital (2%) X3000 SEM

Figure 14. Microstructure of wet drawn wire in New Industrial Trials (Good Drawability)

1998 © 2019 by the Association for Iron & Steel Technology.


Previous Trials- Trial1 Chemical Composition & Early Trials Cooling Patterns 1-4 Microstructure
Pattern Quality Map Area of Brittle Phases (Pink 7%) Pattern Quality Histograms

New Trials- Trial2 Chemical Composition & Optimized Cooling Pattern 6-7 Microstructure
Pattern Quality Map Area of Brittle Phases (Pink <1%) Pattern Quality Histograms

Figure 15. SEM-EBSD analysis of wet drawn wire in Previous Failed Trials (breakage) & New Industrial Trials (good
drawability)
With EBSD method, crystallographic contrast come up with different colors of the gray scale. This helps to separate the
phase ingredients by looking at the pattern quality maps which consist of the information gathered from every single
grain/subgrain in the sample. Differentiations in pattern quality histograms means the differentiations in that/those grain
structure. The pattern quality map scale has a tendency to spread according to the amount of deformation in the structure and
the pattern quality values of the deformed phases converge to ‘0’. Therefore, the low pattern quality values in the histogram
indicate the presence of deformable phases such as martensite and bainite.
Results of the mechanical & chemical properties of the previous failed trials and new trials with good drawability were
shown in Table4.

Table 4. Chemical composition and mechanical properties.

© 2019 by the Association for Iron & Steel Technology. 1999


CONCLUSIONS
In this study, computational and experimental methods were used to identify the root cause of production problems in the
early trials and finally to produce ferritic- perlitic wire rods with good drawability for gas metal arc welding wire applications
that satisfy the customer demands.
Early investigations showed that breakage is associated with the presence of a brittle phases, center star cracks/segregation,
inclusions, insufficient homogeneous slow cooling in Stelmor® line, chemical composition in upper limits, nonhomogeneous
cooling in cooling box. Firstly, some improvements were done in steelmaking, continuous casting sides like optimizing super
heat, cooling in mould sections, EMS (electromagnetic stirring) and more to prevent center star cracks/segregation and
detrimental inclusions. For good drawability and to decrease the segregation levels for removing the brittle phases C-Mn
contents were revised to lower limits also in steelmaking side. C%:0.060-0.074 Mn%: 1.60-1.70, Si%:0.85-0.90 was
determined as optimum amounts.
Later in solution step, it was found that optimization can also be performed in the actual Stelmor® line cooling process to
obtain adequate homogeneous slow cooling to remove brittle phases. To obtain adequate homogeneous slow cooling steel
sheets were added under conveyor, 3 more covers were added in 4th section of the conveyor line and covers positioning was
improved also. Cooling patterns and chemical compositions determined in experimental and computational studies were
applied to Industrial trials to obtain good drawability especially in wet wire drawing process from 2.0 mm to 1.2, 1.0 and 0.8
mm in customer line. Breakages were noticed in customer line while wet drawing process from 2.00 mm to 0.8 mm in
previous trials. However in new trials good drawability were obtained without breakage in wet drawing process from 2.00
mm to 0.8 mm. Optical microscope and SEM, SEM-EBSD analyses of the 5.5mm wire rod and 0.8mm drawn wire verified
the removal of brittle phases after optimizing the chemical composition and process parameters in both steelmaking,
continuous casting and rolling mill side. Also by decreasing C-Mn-Si content average tensile strength in new trials were 11
MPa less than the previous trials which has a positive effect on drawability.

REFERENCES
1. Souvik Dasa, Sandip Thalukdarb, Goutam Mukhopadhyaya, Sandip Bhattacharyaa, Breakage of electrode grade steel
wires during manufacturing: A metallurgical investigation, Engineering Failure Analysis 95 (2019) 199–205
2. Leonard E.Samuels, Light microscopy of carbon steels, p. 258.
3. Sakallı, E., Günbay S., Çelikel A.E., Gül H., Gündüz O.,“Design and Improvement of a High Carbon Steel Wire Rod
Grade for PC Strand Applications”, AISTech2016 Conference, May 16-19, 2016, Pittsburgh, PA, USA.

2000 © 2019 by the Association for Iron & Steel Technology.

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