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ANALYSIS OF THE EFFECT OF ADDITION OF
SILICON CARBIDE TO TITANIUM DIOXIDE
FLUXES IN THE ATIG WELDING OF 304 AND
316L STAINLESS STEELS
BY,
PRASHANTH P (311817145001)
VIJAYA VIGNESH B (311817145002)
4TH YEAR, MATERIAL SCIENCE AND ENGINEERING DEPARTMENT
MOHAMED SATHAK AJ COLLEGE OF ENGINEERING, CHENNAI - 603103
An introduction to TIG welding
 Tungsten Inert Gas (TIG) or Gas Tungsten Arc Welding (GTAW) is an arc welding
process that uses a non-consumable electrode.
 The electrode used is made out of Tungsten.
 Filler metal is added separately into the weld pool.
 A blanket of inert gas, also known as shielding gas is used to protect the weld
from contamination.
Advantages of TIG welding
 The electrode is not consumed during welding.
 Inert gases are used to prevent contamination as opposed to flux.
 Intenesive post weld cleaning is not required due to the absence of flux.
 Welds produced are relatively clean and narrow.
 TIG welding can be used to weld a wide range of metals.
Disadvantges of TIG welding
 The most important disadvantage is the lack of penetration.
 Specimen greater than 3mm require edge preparation.
 TIG welding requires a greater skill level and dexterity since the welder is forced to
use both of their hands.
Increasing penetration depth – (A-TIG)
welding
 The penetration depth in the conventional TIG welding process is very low.
 This disadvantage can be mitigated through the use of an ‘activated flux’.
 The flux is a chemical substance (usually an oxide) that is applied to the joint
interface prior to welding.
 Activated TIG (A-TIG) welding is the name given to a TIG welding process that
makes use of fluxes to increase the penetration depth.
Mechanisms of A-TIG welding – Arc
constriction
 The exact mechanism behind A-TIG welding is not clearly understood.
 One proposed mechanism is the construction of the welding arc.
 The presence of insulating fluxes along the edges of the joint interface constricts
the arc towards the joint interface.
 This increases the electron density at the surface of the base metal thus increasing
the welding current and arc voltage.
Mechanisms of A-TIG welding –
Marangoni convection
 Another proposed mechanism is ‘Marangoni convection’.
 Marangoni convection or reversed convection is the tendency for heat and mass
transfer to occur towards a region of higher surface tension in a liquid.
 Convection in the weld pool in A-TIG welding is reversed resulting in the
formation of a deep and narrow weld zone.
Conventional TIG welding vs A-TIG
welding
 The image shown below illustrates the arc constriction and Marangoni convection
phenomena seen in A-TIG welding.
Beneficial effects of activated fluxes
 In addition to increasing the penetration depth, activated fluxes were found to
improve other material properties in the weldment.
 Researchers have found that some fluxes greatly improved the tensile strength,
hardness and toughness of the weld metal.
 Therefore A-TIG welding could have other benefits in addition to an increase in
penetration depth.
Flux selection – Titanium dioxide and
Silicon Carbide
 The choice of flux for this particular experimental project was Titania and Silicon
Carbide.
 Silicon Carbide powders were used to improve the hardness of the weld metal.
 Titania was used to improve the penetration depth and to act as a carrier for
depositing the Silicon Carbide deep within the weld pool.
 Three compositions of Titania and Silicon Carbide were taken in the ratios 3:1, 2:1
and 1:1.
Material selection – 304 and 316L stainless
steels
 The materials of choice for this experiment were 304 and 316L stainless steel
grades belonging to the austenitic stainless steel family.
 They base materials were chosen based on their weldability.
 The filler metal of choice was ER308L taken in the form of one meter long filler
rods.
Experimental procedure - process flow
The steps involved in the experimental procedure were as follows,
 Sourcing of raw materials and equipment.
 Preparing the base metals for welding.
 Preparation of the flux mixture.
 Application of the flux mixture.
 Welding the specimen.
 Post weld cleaning.
 Preparing the specimen for testing.
 Testing the hardness of the specimen.
 Analysis of the test results.
Sourcing of raw materials and equipment
The raw materials required for this experiment were,
1. 4 pieces of 304 stainless steel (100 mm x 250 mm)
2. 4 pieces of 316L stainless steel (100 mm x 250 mm)
3. ER308L welding rods
4. Titanium (IV) oxide powders (100 g)
5. Silicon Carbide powders (100 g)
6. Acetone (500 ml)
Preparing the base metals for welding
 Prior to welding the specimen surface was cleaned using acetone.
 The edges to be joined were ground using a grinding tool.
 The ground edge of a 304 SS sheet and a 316L SS sheet were lined up in closed
square butt configuration.
 Tack welds were made to hold the sheets in place.
Preparation of the flux mixture
 Titania and Silicon Carbide powders were mixed together in three different ratios
to prepare the flux.
 The ratios of Titania to Silicon Carbide were 3:1, 2:1 and 1:1.
 Acetone was added to flux mixture in a 1:1 ratio by volume.
Application of the flux mixture
 The flux mixture is added to specimen just
before welding.
 The flux is brushed on top of the joint
interface.
 Acentone evaporates leaving behind a thin
layer of flux.
 Four specimens were taken in total – one
specimen without flux (No flux – NF) and
three others with flux coating.
 The given image shows a flux coated
specimen prior to welding.
Welding the specimens
The specimens were welded using the following weld parameters,
 Amperage – 120 A
 Shielding gas – pure argon
 Gas flow rate – 7 l/min
 Electrode – thoriated tungsten (ground to a sharp tip)
 Filler metal - ER308L
 Weld current/ configuration – DCEN
 Joint – Closed square butt joint
Post weld cleaning
 The specimens welded with the flux were cleaned using a wire brush.
 Acetone was used to remove surface contaminants.
 The NF specimen did not require intensive cleaning.
Preparing the specimen for testing
 The weld bead of the specimen was ground using a belt grinder.
 This was done to expose the weld metal underneath.
 The ground regions were cleaned with acetone to remove contaminants.
Testing the hardness of the specimen
 The specimens were subjected to Rockwell hardness tests.
 Rockwell C scale was used.
 Three sets of measurements were made along the weld centre line.
Analysis of the test results
 The readings on the dial were noted and tabulated.
 The average hardness value of each welded sample was determined.
 The hardness values of the specimens were compared with each other.
 Assumptions were made by analysing the results.
Result and Analysis
Hardness values:
 The hardness values of the weld zones of the test specimens in HRC are as follows
No Flux (NF) 3 : 1 2 : 1 1 : 1
18 20 21 21
19 23 24 24
19 20 19 23
Avg : 18.67 ≈ 19 Avg : 21 Avg : 21.33 ≈ 21 Avg : 22.67 ≈ 23
Contd...
 The face side if the welded specimen were
analysed.
 The NF specimen was found to have the
cleanest weld of the four specimen.
 The image given here shows the face side
of the weldments – (clockwise from top
left) No flux (NF) specimen, 3:1 specimen,
2:1 specimen and 1:1 specimen.
Contd...
 The root side of the welded specimens
were analysed.
 The NF specimen was found to have the
least weld penetration of the four
specimen.
 The image given here shows the root side
of the weldments – (clockwise from top
left) No flux (NF) specimen, 3:1 specimen,
2:1 specimen and 1:1 specimen.
Conclusion
The experiment can be concluded through the following points.
 Activated TIG welding was found to be an efficient alternative to TIG welding in
situations where enhanced weld properties such as improved penetration and
hardness are required.
 While the no flux specimen looked aesthetically pleasing, the specimens which
were welded with the addition of the flux showed greater weld penetration.
 For applications where deeper penetration is required, higher percentages of
Titania can be used.
 For applications where harder welds are required, higher percentages of Silicon
Carbide can be used.
References
1. Kumar, Mukesh&Rana, Naveen & Kannan, M.. (2020). Some studies on the performance of
activated-tig welding in steel weldments.
2. Badheka, Vishvesh&Basu, Ritwik&Omale, Joseph &Szpunar, Jerzy. (2016). Microstructural Aspects
of TIG and A-TIG Welding Process of Dissimilar Steel Grades and Correlation to Mechanical
Behavior. Transactions of the Indian Institute of Metals. 69. 10.1007/s12666-016-0836-5.
3. Remenar, Maja &Kožuh, Z. &Garasic, Ivica &Bušić, Matija. (2018). Optimization of the A-TIG
welding for stainless steels. IOP Conference Series: Materials Science and Engineering. 329.
012012. 10.1088/1757-899X/329/1/012012.
4. Roy, Sagar&Samaddar, Siladitya& Uddin, Md &Hoque, Aktarul& Mishra, Sagnik& Das, Santanu.
(2017). Effect of Activating Flux on Penetration in ATIG Welding of 316 Stainless Steel. Indian
Welding Journal. 50. 72. 10.22486/iwj/2017/v50/i4/162275.
5. Kumar, R. &Bharathi, Sundara. (2015). A Review Study on A-TIG Welding of 316(L) Austenitic
Stainless Steel.
Contd...
6. Wu, Hong & Chang, Yunlong & Mei, Qiang & Liu, Dan. (2019). Research advances in high-energy
TIG arc welding. The International Journal of Advanced Manufacturing Technology. 104.
10.1007/s00170-019-03918-5.
7. Hasan, Aysha & Ali, Obed & Alsaffawi, Adnan. (2018). Effect of Welding Current on Weldments
Properties in MIG and TIG Welding. International Journal of Engineering and Technology(UAE). 7.
192-197. 10.14419/ijet.v7i4.37.24099.
8. Çiçek, Bünyamin & Gündoğdu İş, Emine & Gümüş, Emre & Yılmaz, Eren & Topuz, Polat. (2015).
Risks and safety measures in tig welding process.
9. Vora, Jay. (2019). Insights into the Flux-Assisted TIG Welding Processes. 10.1201/9781351234825-
11.
10. Garg, Himanshu & Sehgal, Karan & Lamba, Rahul & Kajal, Gianender. (2019). A Systematic Review:
Effect of TIG and A-TIG Welding on Austenitic Stainless Steel. 10.1007/978-981-13-6412-9_36.
Contd...
11. Mishra, Debashis. (2017). TIG welding.
12. Li, H. & Zou, J.-S & Yao, J.-S & Peng, H.-P. (2018). Activating Flux TIG Welding Technology of 2219
High Strength Aluminum Alloy. Cailiao Gongcheng/Journal of Materials Engineering. 46. 66-73.
10.11868/j.issn.1001-4381.2016.001169.
13. Sehdev, Mayank & Singh, Vikram & Sunny, Kevin & Singh, Yadvinder. (2019). Review and
fabrication of automatic TIG welding machine. 10.13140/RG.2.2.25939.84006.
14. Singh, Nitish. (2019). Numerical Investigation of TIG welding Process using Finite Element Method.
International Journal for Research in Applied Science and Engineering Technology. 7. 733-738.
10.22214/ijraset.2019.1114.
15. Shrivas, Sharda & Vaidya, Sanjay & Khandelwal, Ashish & Vishvakarma, Amit. (2020). Investigation
of TIG welding parameters to improve strength. Materials Today: Proceedings. 26.
10.1016/j.matpr.2020.02.416.
Contd...
16. (2018). Effects of welding parameters on penetration depth in mild steels A-TIG welding. Scientia
Iranica. 10.24200/sci.2018.20145.
17. Ogundimu, Emmanuel & Akinlabi, Esther & Erinosho, Mutiu. (2019). Comparative Study between
TIG and MIG Welding Processes. Journal of Physics: Conference Series. 1378. 022074.
10.1088/1742-6596/1378/2/022074.
18. Vidyarthy, Ravi & Dwivedi, Dheerendra & Vasudevan, M.. (2017). Influence of M-TIG and A-TIG
Welding Process on Microstructure and Mechanical Behavior of 409 Ferritic Stainless Steel. Journal
of Materials Engineering and Performance. 26. 10.1007/s11665-017-2538-5.
19. Saha, Suman & Das, Santanu. (2019). Application of Activated Tungsten Inert Gas (A-TIG) Welding
Towards Improved Weld Bead Morphology in Stainless Steel Specimens.
20. Ouis, Abousoufiane & Djoudjou, Rachid & Abdejlil, Hedhibi & Alrobei, Hussein & Albaijan, Ibrahim
& Alzahrani, Bandar & Sherif, El-Sayed & Abdo, Hany. (2020). Effects of ATIG Welding on Weld
Shape, Mechanical Properties, and Corrosion Resistance of 430 Ferritic Stainless Steel Alloy. Metals
- Open Access Metallurgy Journal. 10. 404. 10.3390/met10030404.

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ATIG welding.pptx

  • 1. ANALYSIS OF THE EFFECT OF ADDITION OF SILICON CARBIDE TO TITANIUM DIOXIDE FLUXES IN THE ATIG WELDING OF 304 AND 316L STAINLESS STEELS BY, PRASHANTH P (311817145001) VIJAYA VIGNESH B (311817145002) 4TH YEAR, MATERIAL SCIENCE AND ENGINEERING DEPARTMENT MOHAMED SATHAK AJ COLLEGE OF ENGINEERING, CHENNAI - 603103
  • 2. An introduction to TIG welding  Tungsten Inert Gas (TIG) or Gas Tungsten Arc Welding (GTAW) is an arc welding process that uses a non-consumable electrode.  The electrode used is made out of Tungsten.  Filler metal is added separately into the weld pool.  A blanket of inert gas, also known as shielding gas is used to protect the weld from contamination.
  • 3. Advantages of TIG welding  The electrode is not consumed during welding.  Inert gases are used to prevent contamination as opposed to flux.  Intenesive post weld cleaning is not required due to the absence of flux.  Welds produced are relatively clean and narrow.  TIG welding can be used to weld a wide range of metals.
  • 4. Disadvantges of TIG welding  The most important disadvantage is the lack of penetration.  Specimen greater than 3mm require edge preparation.  TIG welding requires a greater skill level and dexterity since the welder is forced to use both of their hands.
  • 5. Increasing penetration depth – (A-TIG) welding  The penetration depth in the conventional TIG welding process is very low.  This disadvantage can be mitigated through the use of an ‘activated flux’.  The flux is a chemical substance (usually an oxide) that is applied to the joint interface prior to welding.  Activated TIG (A-TIG) welding is the name given to a TIG welding process that makes use of fluxes to increase the penetration depth.
  • 6. Mechanisms of A-TIG welding – Arc constriction  The exact mechanism behind A-TIG welding is not clearly understood.  One proposed mechanism is the construction of the welding arc.  The presence of insulating fluxes along the edges of the joint interface constricts the arc towards the joint interface.  This increases the electron density at the surface of the base metal thus increasing the welding current and arc voltage.
  • 7. Mechanisms of A-TIG welding – Marangoni convection  Another proposed mechanism is ‘Marangoni convection’.  Marangoni convection or reversed convection is the tendency for heat and mass transfer to occur towards a region of higher surface tension in a liquid.  Convection in the weld pool in A-TIG welding is reversed resulting in the formation of a deep and narrow weld zone.
  • 8. Conventional TIG welding vs A-TIG welding  The image shown below illustrates the arc constriction and Marangoni convection phenomena seen in A-TIG welding.
  • 9. Beneficial effects of activated fluxes  In addition to increasing the penetration depth, activated fluxes were found to improve other material properties in the weldment.  Researchers have found that some fluxes greatly improved the tensile strength, hardness and toughness of the weld metal.  Therefore A-TIG welding could have other benefits in addition to an increase in penetration depth.
  • 10. Flux selection – Titanium dioxide and Silicon Carbide  The choice of flux for this particular experimental project was Titania and Silicon Carbide.  Silicon Carbide powders were used to improve the hardness of the weld metal.  Titania was used to improve the penetration depth and to act as a carrier for depositing the Silicon Carbide deep within the weld pool.  Three compositions of Titania and Silicon Carbide were taken in the ratios 3:1, 2:1 and 1:1.
  • 11. Material selection – 304 and 316L stainless steels  The materials of choice for this experiment were 304 and 316L stainless steel grades belonging to the austenitic stainless steel family.  They base materials were chosen based on their weldability.  The filler metal of choice was ER308L taken in the form of one meter long filler rods.
  • 12. Experimental procedure - process flow The steps involved in the experimental procedure were as follows,  Sourcing of raw materials and equipment.  Preparing the base metals for welding.  Preparation of the flux mixture.  Application of the flux mixture.  Welding the specimen.  Post weld cleaning.  Preparing the specimen for testing.  Testing the hardness of the specimen.  Analysis of the test results.
  • 13. Sourcing of raw materials and equipment The raw materials required for this experiment were, 1. 4 pieces of 304 stainless steel (100 mm x 250 mm) 2. 4 pieces of 316L stainless steel (100 mm x 250 mm) 3. ER308L welding rods 4. Titanium (IV) oxide powders (100 g) 5. Silicon Carbide powders (100 g) 6. Acetone (500 ml)
  • 14. Preparing the base metals for welding  Prior to welding the specimen surface was cleaned using acetone.  The edges to be joined were ground using a grinding tool.  The ground edge of a 304 SS sheet and a 316L SS sheet were lined up in closed square butt configuration.  Tack welds were made to hold the sheets in place.
  • 15. Preparation of the flux mixture  Titania and Silicon Carbide powders were mixed together in three different ratios to prepare the flux.  The ratios of Titania to Silicon Carbide were 3:1, 2:1 and 1:1.  Acetone was added to flux mixture in a 1:1 ratio by volume.
  • 16. Application of the flux mixture  The flux mixture is added to specimen just before welding.  The flux is brushed on top of the joint interface.  Acentone evaporates leaving behind a thin layer of flux.  Four specimens were taken in total – one specimen without flux (No flux – NF) and three others with flux coating.  The given image shows a flux coated specimen prior to welding.
  • 17. Welding the specimens The specimens were welded using the following weld parameters,  Amperage – 120 A  Shielding gas – pure argon  Gas flow rate – 7 l/min  Electrode – thoriated tungsten (ground to a sharp tip)  Filler metal - ER308L  Weld current/ configuration – DCEN  Joint – Closed square butt joint
  • 18. Post weld cleaning  The specimens welded with the flux were cleaned using a wire brush.  Acetone was used to remove surface contaminants.  The NF specimen did not require intensive cleaning.
  • 19. Preparing the specimen for testing  The weld bead of the specimen was ground using a belt grinder.  This was done to expose the weld metal underneath.  The ground regions were cleaned with acetone to remove contaminants.
  • 20. Testing the hardness of the specimen  The specimens were subjected to Rockwell hardness tests.  Rockwell C scale was used.  Three sets of measurements were made along the weld centre line.
  • 21. Analysis of the test results  The readings on the dial were noted and tabulated.  The average hardness value of each welded sample was determined.  The hardness values of the specimens were compared with each other.  Assumptions were made by analysing the results.
  • 22. Result and Analysis Hardness values:  The hardness values of the weld zones of the test specimens in HRC are as follows No Flux (NF) 3 : 1 2 : 1 1 : 1 18 20 21 21 19 23 24 24 19 20 19 23 Avg : 18.67 ≈ 19 Avg : 21 Avg : 21.33 ≈ 21 Avg : 22.67 ≈ 23
  • 23. Contd...  The face side if the welded specimen were analysed.  The NF specimen was found to have the cleanest weld of the four specimen.  The image given here shows the face side of the weldments – (clockwise from top left) No flux (NF) specimen, 3:1 specimen, 2:1 specimen and 1:1 specimen.
  • 24. Contd...  The root side of the welded specimens were analysed.  The NF specimen was found to have the least weld penetration of the four specimen.  The image given here shows the root side of the weldments – (clockwise from top left) No flux (NF) specimen, 3:1 specimen, 2:1 specimen and 1:1 specimen.
  • 25. Conclusion The experiment can be concluded through the following points.  Activated TIG welding was found to be an efficient alternative to TIG welding in situations where enhanced weld properties such as improved penetration and hardness are required.  While the no flux specimen looked aesthetically pleasing, the specimens which were welded with the addition of the flux showed greater weld penetration.  For applications where deeper penetration is required, higher percentages of Titania can be used.  For applications where harder welds are required, higher percentages of Silicon Carbide can be used.
  • 26. References 1. Kumar, Mukesh&Rana, Naveen & Kannan, M.. (2020). Some studies on the performance of activated-tig welding in steel weldments. 2. Badheka, Vishvesh&Basu, Ritwik&Omale, Joseph &Szpunar, Jerzy. (2016). Microstructural Aspects of TIG and A-TIG Welding Process of Dissimilar Steel Grades and Correlation to Mechanical Behavior. Transactions of the Indian Institute of Metals. 69. 10.1007/s12666-016-0836-5. 3. Remenar, Maja &Kožuh, Z. &Garasic, Ivica &Bušić, Matija. (2018). Optimization of the A-TIG welding for stainless steels. IOP Conference Series: Materials Science and Engineering. 329. 012012. 10.1088/1757-899X/329/1/012012. 4. Roy, Sagar&Samaddar, Siladitya& Uddin, Md &Hoque, Aktarul& Mishra, Sagnik& Das, Santanu. (2017). Effect of Activating Flux on Penetration in ATIG Welding of 316 Stainless Steel. Indian Welding Journal. 50. 72. 10.22486/iwj/2017/v50/i4/162275. 5. Kumar, R. &Bharathi, Sundara. (2015). A Review Study on A-TIG Welding of 316(L) Austenitic Stainless Steel.
  • 27. Contd... 6. Wu, Hong & Chang, Yunlong & Mei, Qiang & Liu, Dan. (2019). Research advances in high-energy TIG arc welding. The International Journal of Advanced Manufacturing Technology. 104. 10.1007/s00170-019-03918-5. 7. Hasan, Aysha & Ali, Obed & Alsaffawi, Adnan. (2018). Effect of Welding Current on Weldments Properties in MIG and TIG Welding. International Journal of Engineering and Technology(UAE). 7. 192-197. 10.14419/ijet.v7i4.37.24099. 8. Çiçek, Bünyamin & Gündoğdu İş, Emine & Gümüş, Emre & Yılmaz, Eren & Topuz, Polat. (2015). Risks and safety measures in tig welding process. 9. Vora, Jay. (2019). Insights into the Flux-Assisted TIG Welding Processes. 10.1201/9781351234825- 11. 10. Garg, Himanshu & Sehgal, Karan & Lamba, Rahul & Kajal, Gianender. (2019). A Systematic Review: Effect of TIG and A-TIG Welding on Austenitic Stainless Steel. 10.1007/978-981-13-6412-9_36.
  • 28. Contd... 11. Mishra, Debashis. (2017). TIG welding. 12. Li, H. & Zou, J.-S & Yao, J.-S & Peng, H.-P. (2018). Activating Flux TIG Welding Technology of 2219 High Strength Aluminum Alloy. Cailiao Gongcheng/Journal of Materials Engineering. 46. 66-73. 10.11868/j.issn.1001-4381.2016.001169. 13. Sehdev, Mayank & Singh, Vikram & Sunny, Kevin & Singh, Yadvinder. (2019). Review and fabrication of automatic TIG welding machine. 10.13140/RG.2.2.25939.84006. 14. Singh, Nitish. (2019). Numerical Investigation of TIG welding Process using Finite Element Method. International Journal for Research in Applied Science and Engineering Technology. 7. 733-738. 10.22214/ijraset.2019.1114. 15. Shrivas, Sharda & Vaidya, Sanjay & Khandelwal, Ashish & Vishvakarma, Amit. (2020). Investigation of TIG welding parameters to improve strength. Materials Today: Proceedings. 26. 10.1016/j.matpr.2020.02.416.
  • 29. Contd... 16. (2018). Effects of welding parameters on penetration depth in mild steels A-TIG welding. Scientia Iranica. 10.24200/sci.2018.20145. 17. Ogundimu, Emmanuel & Akinlabi, Esther & Erinosho, Mutiu. (2019). Comparative Study between TIG and MIG Welding Processes. Journal of Physics: Conference Series. 1378. 022074. 10.1088/1742-6596/1378/2/022074. 18. Vidyarthy, Ravi & Dwivedi, Dheerendra & Vasudevan, M.. (2017). Influence of M-TIG and A-TIG Welding Process on Microstructure and Mechanical Behavior of 409 Ferritic Stainless Steel. Journal of Materials Engineering and Performance. 26. 10.1007/s11665-017-2538-5. 19. Saha, Suman & Das, Santanu. (2019). Application of Activated Tungsten Inert Gas (A-TIG) Welding Towards Improved Weld Bead Morphology in Stainless Steel Specimens. 20. Ouis, Abousoufiane & Djoudjou, Rachid & Abdejlil, Hedhibi & Alrobei, Hussein & Albaijan, Ibrahim & Alzahrani, Bandar & Sherif, El-Sayed & Abdo, Hany. (2020). Effects of ATIG Welding on Weld Shape, Mechanical Properties, and Corrosion Resistance of 430 Ferritic Stainless Steel Alloy. Metals - Open Access Metallurgy Journal. 10. 404. 10.3390/met10030404.