Engineering, Technology & Applied Science Research Vol. 9, No. 2, 2019, 3990-3997 3990

www.etasr.com Touileb et al.: Mixing Design for ATIG Morphology and Microstructure Study of 316L Stainless Steel

Mixing Design for ATIG Morphology and

Microstructure Study of 316L Stainless Steel

Kamel Touileb

Mechanical Engineering Department,

College of Engineering, Prince Sattam

Bin Abdulaziz University,

Al Kharj, Saudi Arabia

k.touileb@psau.edu.sa

Abdejlil Hedhibi

Mechanical Engineering Department,

College of Engineering, Prince Sattam

Bin Abdulaziz University,

Al Kharj, Saudi Arabia

a.hedhibi@psau.edu

Rachid Djoudjou

Mechanical Engineering Department,

College of Engineering, Prince Sattam

Bin Abdulaziz University,

Al Kharj, Saudi Arabia

r.djoudjou@psau.edu.sa

Abousoufiane Ouis

Mechanical Engineering Department,

College of Engineering, Prince Sattam Bin Abdulaziz

University, Al Kharj, Saudi Arabia

a.ouis@psau.edu.sa

Mohamed Lamjed Bouazizi

Mechanical Engineering Department,

College of Engineering, Prince Sattam Bin Abdulaziz

University, Al Kharj, Saudi Arabia

my.bouazizi@psau.edu.sa

Abstract—This work is a study of the effects of oxides

combination on the morphology of 316L stainless steel welds. A

series of thirteen weld lines were carried out using thirteen

different oxides. Based on the depth and ratio D/W results, three

candidate oxides were selected: Ti2O, Mn2O3, and SiO2. Mixing

method available in Minitab 17 software is the most appropriate

method to find the optimal combinations to get the best depth

and D/W ratio. According to simplex lattice degree four, nineteen

combinations of these oxides were prepared. The results show

that the optimal composition of flux was: 66%SiO2-34% Mn2O3.

The depth and D/W ratio increased to 8.85mm and 0.98

respectively for optimal ATIG, whereas for the conventional TIG

welding, the depth and the ratio D/W didn't exceed 1.65mm and

0.17 respectively. For TIG weld joint the hardness is about 47

HRA and it increases to 77 HRA for the optimal ATIG weld

joint. The absorbed energies in Charpy impact test are 146 and

138kJ in the weld zone and in the heat affected zone respectively

for the TIG welding and they dropped to 111 and 74kJ for the

optimal ATIG welding. The fracture surface examined by

scanning electron microscope (SEM) shows a ductile fracture for

TIG weld with small dimples but ductile-brittle fracture for

ATIG weld. Energy dispersive spectroscopy (EDS/SEM) analysis

shows the formation of FeS2 and SiO2 in the weld zone causing

low absorbed energy for ATIG weld.

Keywords-ATIG; 316L austenitic stainless steel; ATIG welding

mixing method; ternary flux

I. INTRODUCTION

TIG welding process is quite widespread. However, weld
penetration varies from cast to cast and the maximum weld
depth in a single pass does not exceed 3mm. Activated TIG
(ATIG) welding proposed by Paton Institute-Kiev [1, 2] seems
an appropriate process to overcome these weaknesses. ATIG
welding uses the same equipment as TIG except a prior weld
operation layer of activated flux paste is deposited on the

workpiece. Hypotheses have been made to explain the
phenomenon favoring a high weld depth. Authors in [3-6]
proposed that the Marangoni convection is the most important
factor in determining weld shape. Surfactant elements as S, Se,
Te, O in weld pool affect the convection of molten metal
leading to centripetal circulation of weld metal getting a depth
of weld. Authors in [7, 8] applied the principle of electron
absorption [9], electronegative elements as halides (fluorine)
migrate to arc weld and capture outer arc electrons which
contribute to contract the arc welding. This phenomenon
increases the density of arc welding and the heat provided to
weld pool. Authors in [10-12] proposed that high electrical
resistance of flux components contributes to arc constriction.
Many works were subsequently carried out using oxides like
SiO2, TiO2, Cr2O3, Fe2O3, CaO, ZrO2, MgO [13-24], chlorides
[25-27], and fluorides [28, 29] to improve weld depth. These
studies showed an increasing in the weld depth without
affecting the mechanical properties of the specimens [30, 31].
Other studies were dedicated to microstructure and mechanical
properties [32-33]. In this work, 13 oxides were investigated on
316L austenitic stainless steel. Design of experiments was used
to predict the best combination of the tested oxides. Mixing
method based on a simplex lattice degree four was the key tool
to optimize the flux combination in order to enhance the depth
and D/W ratio.

II. EXPERIMENTAL PROCEDURE

A. Materials

The material used was the 316L stainless steel whose
chemical composition is shown in Table I. Experiments
consisted of welding a 20cm line on a rectangular plate of 6mm
thickness. Before welding, the plates were cleaned with
acetone. Flux powders were dried in furnace to eliminate
humidity, and then mixed with methanol in 1:1 ratio. A flux

Corresponding author: Kamel Touileb

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layer less than 0.2mm thick was deposited on the surface to be
welded.

TABLE I. 316L CHEMICAL COMPOSISTION

Element Percentage (%)

C 0.018

Mn 1.30

Si 0.43

P 0.034

S 0.0029

Cr 16.78

Ni 10.00

Mo 2005

Ti 0.0042

Cu 0.2082

Co 0.226

N (ppm) 321

B. Welding Procedure

A Tungsten Inert Gas welding machine was used. A water-
cooled torch with a standard 2% thoriated tungsten electrode
rod having diameter of 3.2mm has been used for the
experiments. The torch was mounted on a motorized carriage
as shown in Figure 1. A series of tests were carried out with
150A welding current and 15cm/min welding speed leading to
a provided energy of 540kJ/m. The welding parameters for the
TIG welding are listed in Table II.

Fig. 1. Experimental setup of TIG welding with flux paste (a motorized
carriage, torch–workpiece).

TABLE II. WELDING PARAMETERS

Welding speed 15cm/min

Welding current 150A

Arc length 2mm

Electrode Tip Angle 45 ͦ

Shield gas on work piece Argon with flow rate 12l/min

Shield gas back side Argon with flow rate 5l/min

Welding mode Direct current electrode negative

C. Mechanical Testing

After welding, the samples were cut as shown in Figure 2 to
acquire test samples for mechanical testing and weld
morphology. The Rockwell hardness measurement was
performed with a Digital Hardness Tester Model HRS-150.
The hardness tests were conducted in the bulk of weld bead,
and the results were the average of four indentations as shown
in Figure 3.

Fig. 2. Different test specimens on welded TIG and ATIG plate

Fig. 3. Hardness test locations on weld bead

Impact tests were carried out with the impact testing
machine model JBS-500. The specimens were cut according to
ASTM E23 and the impact tests were conducted in the weld
bead and in the HAZ as shown in Figure 4.

(a)

(b)

Fig. 4. Test specimen for impact test (a) weld zone, (b) HAZ

D. Experiment by Mixing Method Design (DOE)

For the DOE, mixing method in mini tab 17 was applied
and consequently the number of experiments to be conducted
was reduced. In order to compare the effect of the flux on the
tensile strength, 13 oxides (SiO2, TiO2, Fe2O3, Cr2O3, ZnO,
ZrO2, CaO, Mn2O3, V2O5, MoO3, SrO2, CoO3, and MgO) were

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tested. Among these oxides, 3 gave the best depth and D/W
ratio and were selected to be used in the mixing design method.
Based on the simplex lattice degree four designs, 19
combinations have been selected. Nineteen weld lines were
executed and samples for morphology, hardness and impact
tests were cut. The optimizer module available in mini tab 17
was used to get the optimal formulation of flux which is
expected to give the best depth and D/W ratio of weld. Finally,
using the optimal formulation, ATIG weld line has been carried
out along with another weld line without flux (TIG).

III. RESULTS AND DISCUSSION

A. Depth D and D/W Ratio

Figure 5 shows the weld depth results of ATIG weldment of

the tested preliminary 14 oxides. The highest value of depth is

6.04mm which is obtained for the sample welded with Mn2O3

flux, followed by the sample welded with SiO2 flux (5.29mm),

and then by the sample welded with TiO2 (4.81mm). So the

oxides Mn2O3, SiO2, and TiO2 were selected. The results of the

depth and D/W ratio for different proportions of the 3 selected

oxides are shown in Table III.

Fig. 5. Depth of ATIG welds.

TABLE III. DIFFERENT COMPOSITIONS OF FLUXES, DEPTH AND D/W

Exp. No. SiO2 % TiO2 % Mn2O3 % Depth (mm) D/W

1 75 25 0 4.23 0.54

2 75 0 25 6.72 0.92

3 0 75 25 4.47 0.58

4 25 75 0 4.61 0.61

5 25 0 75 3.77 0.49

6 0 25 75 3.95 0.53

7 0 50 50 5.66 0.77

8 50 0 50 6.63 0.90

9 50 50 0 6.36 0.83

10 50 25 25 6.66 0.86

11 25 50 25 4.85 0.63

12 25 25 50 3.48 0.43

13 33.3 33.3 33.3 4.93 0.66

14 66.67 16.67 16.67 5.01 0.72

15 16.67 66.67 16.67 5.27 0.72

16 16.67 16.67 66.67 4.70 0.64

17 100 0 0 5.29 0.74

18 0 100 0 4.81 0.66

19 0 0 100 6.04 0.82

B. Mixture Contour Plot

Mixture contour plots for depth D and D/W were generated
using Minitab software and are shown in Figure 6. The iso-
contour lines and the regions confined between them indicate
different levels of depth or D/W. Different colors represent the

different levels of the two properties. The interesting zone lies
where the values of depth and D/W were higher. Optimizer
module available in Minitab was used to predict the responses
of depth and D/W ratio. The composite desirability is equal to 1
(100%). It indicates that the parameters achieve favorable
results for all responses, which means that both responses are
within acceptable limits, as shown in Figure7. The predicted
values are listed in Table IV. The optimal combination of flux
is represented in Table V.

(a)

(b)

Fig. 6. Mixture contour of plot for (a) Depth and (b) D/W ratio.

Fig. 7. Optimization plot

TABLE IV. PREDICTED RESPONSES (UTS, HRA) OF WELD EXECUTED
WITH OPTIMAL FLUX

Responses Predicted responses Desirability

Depth(mm) 7.01 100%

D/W 0.96 100%

TABLE V. OPTIMAL COMPOSITION OF FLUX.

variables SiO2 TiO2 Mn2O3

Percentage (%)s
66 0 34

100

C. Confirmation Test

The confirmation test is the last step in the experimental
process. Confirmation tests were conducted based on the
optimum flux composition obtained in the mixing design
method of Minitab. The experimental values of depth and D/W
ratio of the optimal flux ATIG weld are reported in Table VI.

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The results show the depth of optimized flux is greater than
TIG weld by 5 times. The ratio D/W improved 6 times. The
experimental values obtained for depth in ATIG and TIG welds
are shown in Figure 8. The penetration weld of optimized flux
(8.85mm) is greater than the maximum value predicted by the
software (7.01mm). Furthermore, the D/W value obtained for
ATIG weld (0.98) is very close to the maximum predicted
value of 0.96 as shown in Figure 9. TIG molten metal behaves
as pure metal with centrifugal convection leading to wide and
sallow weld bead contrariwise. ATIG weld metal has a
centripetal movement related to oxygen liberated from oxides
during welding operation. The quantity of liquid melted in
ATIG (51.51mm2) is higher than in TIG weld bead (14.2mm2)
as shown in Figures10-11.

TABLE VI. MORPHOLOGY OF TIG AND ATIG WELDS.

ATIG(with optimal flux) TIG

Depth(mm) 8.85 1.65

W(mm) 9.04 9.92

D/W 0.98 0.17

Fig. 8. Depths of ATIG and TIG welds

Fig. 9. D/W of ATIG and TIG welds

Fig. 10. Areas of ATIG and TIG welds

D. Hardness Test

The experimental values obtained for hardness are shown in
Figure 12. ATIG hardness number of HRA=77 is greater than
TIG hardness number of HRA=47.

(a)

(b)

Fig. 11. Morphology of (a) ATIG and (b) TIG welds

Fig. 12. Hardness HRA in weld zone for ATIG and TIG welds.

E. Impact Test

The experimental values obtained from the impact test are
shown in Figures 13-14.

Fig. 13. Absorbed energy in weld zone for TIG and ATIG welds.

Fig. 14. Absorbed energy in HAZ for TIG and ATIG welds.

The energies absorbed either in the weld zones or in HAZ
of TIG welds are higher than the ones of ATIG welds. Figure
15 shows the images of fractograph of the “V” notch Charpy

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impact test conducted on scanning electronic microscope
(SEM). The images show the formation of micro-voids, with
multiple dimples which demonstrate that the fracture is in
ductile mode in the cases of TIG weld zone (a) and in TIG heat
affected zone (c). Combined ductile (small colonies with finer
dimples) and brittle fracture mode formation characterizes the
ATIG weld zone (b) and the ATIG affected zone (d). The
combined ductile and brittle fracture mode leads to poor
resistance to sudden impact loads.

(a) TIG welded
zone (500X )

(b) ATIG
welded zone

(500X )

(500X)

(d) ATIG heat
affected zone

(500X)

Fig. 15. Fractograph of SS 316L impact charpy “V” notch

F. Microstructure Study

Microstructure study was performed in order to view the
material properties after the welding in both TIG and ATIG
weldings.

1) EDS/SEM Analysis

The results of EDS/SEM analysis in Figures 16 and 17
show the presence of silicon, sulphur and oxygen in ATIG
weld bead and in the heat affected zone, that lead to formations
of inclusions as FeS2. Moreover, oxygen initiates microvoids
and propagates by micro void coalescence, which facilitate the
fracture phenomenon. These results can explain the low impact
resistance in ATIG weld. The results of EDS/SEM analysis in
Figures 18 and 19 show the presence of silicon in TIG weld
zone in quantities close to the quantity in the received plate.
The weld zone and the HAZ are free from oxygen and sulphur
which can explain the withstanding of TIG weld to sudden
impact. The results obtained with EDS/SEM regarding TIG
weld may explain the high resistance to impact test.

Fig. 16. EDS/SEM spectrum analysis of fracture face of ATIG welded zone

Fig. 17. EDS/SEM spectrum analysis of fracture face of ATIG HAZ

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TABLE VII. ELEMENTS PRESENT IN FRACTURE FACE OF ATIG
WELDED ZONE

Element C Si Cr Mn Fe Ni O S

Weight% 20.50 0.51 14.43 1.98 53.44 6.41 2.29 0.43

TABLE VIII. ELEMENTS PRESENT IN FRACTURE FACE OF ATIG HAZ

Element C Si Cr Mn Fe Ni O S

Weight % 21.17 0.56 14.57 1.43 52.93 6.57 2.36 0.42

The results of EDS/SEM analysis in Figures 18 and 19
show the presence of silicon in TIG weld zone. The weld zone
and the HAZ are free from oxygen and sulphur which can
explain the widstand of TIG weld to sudden impact. The results
obtained with EDS/SEM regarding TIG weld may explain the
high resistance to impact test.

Fig. 18. EDS/SEM spectrum analysis of fracture face of TIG welded zone

TABLE IX. ELEMENTS PRESENT IN FRACTURE FACE OF TIG WELDED
ZONE

Element C Si Cr Fe Ni

Weight% 21.23 0.48 14.52 56.32 7.44

Fig. 19. EDS/SEM spectrum analysis of fracture face of TIG HAZ

TABLE X. ELEMENTS PRESENT IN FRACTURE FACE OF TIG HAZ

Element C Cr Fe Ni

Weight% 44.04 7.06 36.10 12.81

2) Ferrite Proportions

The measurement of ferrite content in the austenite matrix
was conducted using area image processing software of
Microvision Instruments. The weld zone appearance of ATIG
and TIG was examined by SEM. The measurements were taken
in 4 different locations in the weld zone and the results were
the average of these measurements. Delta ferrite morphology
has a vermicular network structure in both ATIG and TIG
welds as shown in Figure 20. Results show ferrite content equal
to 10.4% for ATIG. Instead, there is a decrease in ferrite
content to 6.8% for TIG. This can be explained by the fact that
in the case of ATIG operation, the weld bead is fully penetrated
with a large weld bead area up to 55mm2. During ATIG weld
operation, the activated flux has a beneficial effect in
increasing the heat provided to weld pool and consequently the
peak temperature in ATIG weld is greater comparatively to
TIG weld leading to increase the proportion of delta ferrite
retained in austenite matrix. On the other hand, in TIG welding,
the bead is wide and shallow so the cooling rate is high. As the
cooling rate is fast the transformation of delta ferrite to
austenite is not completed, resulting on the presence of delta
ferrite in the weld bead.

(a) Delta ferrite

in ATIG weld
zone

(FN=10.4%)

(b) Delta
ferrite in TIG

weld zone

(FN=6.8%)

Fig. 20. SEM micrograph of (a) ATIG weld zone and (b) TIG weld zone.
Magnification 250X

The ferrite content in heat affected zone is up to 4.6% in
ATIG welding and decreases at 1.4% in TIG heat affected
zone. In TIG, the delta ferrite is randomly distributed in
globular form or in small slats as shown in Figure 21(b).
However, in ATIG heat affected zone, delta ferrite looks-like
elongated inclined stringers as shown in Figure 21(a).

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(a) Delta ferrite in

ATIG HAZ
(FN=4.6%)

(b) Delta ferrite in
TIG HAZ (FN=1.4%)

Fig. 21. SEM micrograph of (a) ATIG HAZ and (b) TIG HAZ.
Magnification 1000X

IV. CONCLUSION

This study was conducted on ATIG welding of austenitic
316L. The results are summarized as follows:

• Among 13 oxides tested, SiO2, TiO2 and Mn2O3 present the
highest depth penetration.

• The optimal flux is composed of 66% SiO2 and 34%
Mn2O3.

• The size of ATIG weld bead is bigger than the one of TIG
weld bead. The activated flux enhances the heat provided to
the weld pool leading to high proportion of retained delta
ferrite (10.4%). However, TIG weld is wider and shallower
so the molten metal cools rapidly in comparison with ATIG
molten metal. In the case of TIG weld the transformation of
delta ferrite to austenite is stopped earlier due to the fast
cooling giving delta ferrite proportions up to 6.8%.

• The hardness HRA property of ATIG weld is improved
comparatively to TIG weld. This result is related with the
high delta ferrite content in ATIG weld zone.

• EDS/SEM analysis reveals the presence of FeS2, silicon,
and oxygen in ATIG welded zone which could be the
reason of the decrease of sudden impact load in comparison
with TIG weld.

• Mixing design method is the more appropriate tool to get
optimal flux composition when depth and D/W ratio
improvements are desirable. Based on experiments’ results,
one can say that Minitab software can predict accurately the
responses.

ACKNOWLEDGEMENTS

This work is supported by the Deanship of Scientific
Research in Prince Sattam Bin Abdulaziz University, Saudi

Arabia under the research project number 2017/01/7373.
Authors acknowledge and thank Dr. Nabeel Alharthi, Director,
Centre of Excellence for Research in Engineering Materials for
his help in performing SEM/EDS analysis.

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