Journal of Metallurgy

Journal of Metallurgy / 2013 / Article

Research Article | Open Access

Volume 2013 |Article ID 827491 | https://doi.org/10.1155/2013/827491

Ajay Kumar, Hari Singh, Sachin Maheshwari, "XRD and DTA Analysis of Developed Agglomerated Fluxes for Submerged Arc Welding", Journal of Metallurgy, vol. 2013, Article ID 827491, 8 pages, 2013. https://doi.org/10.1155/2013/827491

XRD and DTA Analysis of Developed Agglomerated Fluxes for Submerged Arc Welding

Academic Editor: Gerhard Sauthoff
Received21 Dec 2012
Revised09 Feb 2013
Accepted11 Feb 2013
Published11 Mar 2013

Abstract

A unique study of structural and chemical analysis of crystalline phases in developed agglomerated fluxes was carried out. Thirty-two fluxes were developed by using a mixture of oxides, halides, carbonates, silicates, and ferroalloys for submerged arc welding. The present paper focuses on only ten (out of thirty-two) fluxes which were analyzed by X-ray diffraction (XRD) to know the different types of oxides formed and changed in oxidation number of metallic centers after sintering process at around 850C. To know the effect of temperature over phase transformation and melting of different compounds, differential thermal analysis (DTA) was carried out from 1000 to 1400C. This study aims to know the quantity of ions present (percentage) and melting behavior of developed agglomerated fluxes for submerged arc welding process.

1. Introduction

The agglomeration method is used for flux preparation by using a mixture of oxides, halides, carbonates, silicates, and ferroalloys [1]. The chemistry of weld metal is always governed by the electrochemical changes at the weld pool flux interface because the important properties of submerged arc welding fluxes are the function of their physiochemical properties [25]. The important chemical reactions take place during heating of ceramic oxide which is the chemical reaction among the different phases [6], phase transformation of minerals [7], formation of crystalline phases [8], and chemical and structural characterization of crystalline phases in agglomerated fluxes for submerged arc welding were observed [9]. Therefore, the developed agglomerated fluxes can be analyzed to know their crystal structure observed during the rise of temperature. The objective of this analysis is to know the crystalline phases as well as to quantify the different types of ions and their distribution in developed agglomerated fluxes (AGF1101–AGF1110) by X-ray diffraction (XRD) and differential thermal analysis (DTA) is used to know the peaks of endothermic temperatures.

2. Experimentation

In the present study, the fluxes have been designed on the basis of binary and ternary phase diagrams for different oxide and fluoride systems [10] and formulated by using response surface methodology technique [11, 12]. In these fluxes, varying amount of oxides and fluorides were added to know the crystalline phases as well as to quantify the different types of ions and their distribution in developed agglomerated fluxes (AGF1101–AGF1110) by X-ray diffraction (XRD) and differential thermal analysis (DTA) was carried out to know the peaks of endothermic temperatures.

CaO-Al2O3-SiO2-based flux systems have been selected for the study as these are the most widely used fluxes at the commercial level. The details of basic constituents, alloying constituents, and their percentage in the developed agglomerated fluxes are reported in Table 1.


Basic constituents and alloying constituentsCaOSiO2Al2O3MnOCaF2MgONiOFe-Cr

Amount (wt %)2035105–1010–205–150–100–10

After ascertaining the compositions and constituents of fluxes, they were prepared by agglomeration method by taking small batches (2 kg) of weighed quantities of powdered chemicals except binder and thoroughly mixed in a ball miller. The prepared granular flux was dried and baked in an electrically heated furnace for 3 hrs at . The dried flux was allowed to cool down to room temperature before storing it in a moisture free box. The XRD analysis was carried out by diffractometer with the monochromatic light wavelength 1.540600  (Cu K ) for all developed agglomerated flux. The DTA was carried out in an Al2O3 crucible from 28 to at the heating rate of /min. Alumina was used as a standard reference for differential thermal analysis.

3. Result and Discussion

3.1. XRD and DTA Analysis of Developed Agglomerated Fluxes

The XRD results of developed agglomerated fluxes are shown in Figures 1, 2, 3, 4, 5, 6, 7, 8, 9, and 10 and by these graphs, it has been observed that a number of crystalline phases are formed due to chemical interaction among ions with potassium silicate binder. The oxides like MnO, MgO, SiO2, Al2O3, and CaO were found in compound form, which means they do not react with one another. The names of different crystalline phases observed in XRD analysis along with their crystal structure were given in Table 2. The quantity of different oxides shown in Table 3 was based on XRD peaks with high intensity [13]. The development of different types of silicates and oxides is mainly due to mixing of potassium silicate during the agglomeration process.


Flux numberCrystalline phaseCrystal structure

AFG1101 (Dmisteinbergite)Hexagonal
AFG1101 (Protoanthrophyllite)Orthorhombic
AFG1101  
AFG1104
O) (Epistilbite)Triclinic
AFG1101 (Palygorskite)Monoclinic
AFG1101Ca2Fe+++(Fe+++, Al)2 (Julgoldite)Monoclinic
AFG1102 (Svyatoslavite)Monoclinic
AFG1102K2CaMg2(Al, Si)36 H2O (Mazzite)Hexagonal
AFG1102  
AFG1103  
AFG1104
Mg2(Al, Fe+++)3Si3AlO10(OH)8 (Sudoite) Monoclinic
AFG1102 (Leucophoenicite)Monoclinic
AFG1102Ca3Al2 ( = 0.2–1.5) (Hibschite)Isometric
AFG1104KAl2(Si3Al)O10(OH, F)2 (Muscovite)Monoclinic
AFG1104  
AFG1107  
AFG1108
(OH) (Manganbabingtonite)Triclinic
AFG1103  
AFG1110
(Juanite)Orthorhombic
AFG1105  
AFG1109
)2 (Tilleyite)Monoclinic
AFG1104  
AFG1108
Mg9(SiO4)4(OH,  F)2 (Hydroxyl clinotumite)Monoclinic
AFG1108 Ca7(SiO4)3(OH)2 (Chegemite)Orthorhombic
AFG1110 Ca14 (Mn++)14Si24O58 (H2O) (Truscottite)Triclinic
AFG1110 (Fe++, Mg, Fe+++)3Si4Al4O10 (H2O) (Ferrosaponite)Monoclinic
AFG1110 (Fukalite)Orthorhombic
AFG1105 2 (Chondrodite)Monoclinic


Serial numberOxidesQuantity of oxides present (wt.%) in developed agglomerated fluxes
AFG1101AFG1102AFG1103AFG1104AFG1105AFG1106AFG1107AFG1108AFG1109AFG1110

1CaO8.2912.4828.105.7611.479.334.8917.2114.6524.53
2 SiO258.8031.1642.385.7121.1938.5721.7931.2712.6533.12
3 Al2O310.5022.9414.3018.2924.1816.6611.3223.3920.003.27
4 MgO7.803.378.1214.4729.786.595.7817.3418.523.37
5 MnO0.0214.291.862.321.8521.20
6 NiO0.02
7 FeO0.910.260.440.893.910.780.634.20
8 Fe2O36.470.580.643.373.482.791.73
9 Na2O0.040.48
10 CO25.417.826.3113.572.15
11 MnO216.66

The curves of differential thermal analysis (DTA) are shown in Figures 11, 12, 13, 14, 15, 16, 17, 18, 19, and 20 and it shows that most of the oxides were stable oxides up to . The ranges of DTA curves were found between 1000 to . With a few exceptions, most of the reactions were endothermic in nature and the endothermic peaks were observed at different temperatures for different fluxes given in Table 4. The endothermic peaks were different for different fluxes because of their different chemical compositions. These endothermic peaks were comparable with the melting reaction of different crystalline phases for different fluxes. In some DTA curves, a zigzag behavior was observed due to gassing or blistering of the glass formation [14]. The anions generally present in the fluxes are and . The cations from the flux like , , , , , , , , and can react with oxygen and tetrahedral unit from the silicates formed in the fluxes. Since, calcium and magnesium ions have the largest negative heat of formation energy , therefore, they react quickly with oxygen in the welding arch. There were changes in oxidation number in some cationic constituents like , , , and . In most of the fluxes, calcium was present which increases the stability of electric arc during welding. The viscosity of fluxes increases by the presence of corundum and SiO2 which are present in most of the fluxes. In most of the fluxes, it has been observed that the MnO and SiO2 are jointly present and increase the thermomechanical behavior of weld joint.


FluxPeaks of endothermic temperature (°C)

AGF11011239.89
AGF11021234.25
AGF11031233.58
AGF11041240.77
AGF11051226.99
AGF11061334.85
AGF11071244.58
AGF11081191.77
AGF11091245.84
AGF11101248.37

4. Conclusion

The study identified the quantity of different ions present in the weld pool, and it also helps to know the different types of oxides and probable crystalline phases in developed agglomerated fluxes during submerged arc welding. Such types of studies are very much helpful to know the effect of compositions of fluxes on thermomechanical behavior of weld metal.

References

  1. J. E. Indacochea, M. Blander, and S. Shah, “Submerged arc welding: evidence for electrochemical effects on the weld pool,” Welding Journal, vol. 68, no. 3, pp. 77–79, 1989. View at: Google Scholar
  2. C. E. Jackson, “Submerged-arc welding, fluxes and relations among process variables,” in Metals Hand Book, pp. 73–77, ASM, Metals Park, Ohio, USA, 1982. View at: Google Scholar
  3. G. G. Wittstock, “Selecting submerged arc fluxes for carbon and low alloy steels,” Welding Journal, vol. 55, pp. 733–741, 1976. View at: Google Scholar
  4. A. M. Paniagua-Mercado, V. M. López-Hirata, and M. L. Saucedo Muñoz, “Influence of the chemical composition of flux on the microstructure and tensile properties of submerged-arc welds,” Journal of Materials Processing Technology, vol. 169, no. 3, pp. 346–351, 2005. View at: Publisher Site | Google Scholar
  5. P. Kanjilal, T. K. Pal, and S. K. Majumdar, “Combined effect of flux and welding parameters on chemical composition and mechanical properties of submerged arc weld metal,” Journal of Materials Processing Technology, vol. 171, no. 2, pp. 223–231, 2006. View at: Publisher Site | Google Scholar
  6. S. S. Singer, Industrial Ceramics, Chapman & Hall, London, UK, 1963.
  7. A. W. Allen, “Optical microscopy in ceramic engineering,” in Proceedings of the 3rd Berkeley International Materials Conference, Berkeley, Calif, USA, June 1966. View at: Google Scholar
  8. R. H. Redwine and M. A. Conrad, “Microstructures developed in crystallized glass ceramics,” in Proceedings of the 3rd Berkeley International Materials Conference, Berkeley, Calif, USA, July 1961. View at: Google Scholar
  9. A. M. Paniagua-Mercado, P. Estrada-Diaz, and V. M. López-Hirata, “Chemical and structural characterization of the crystalline phases in agglomerated fluxes for submerged-arc welding,” Journal of Materials Processing Technology, vol. 141, no. 1, pp. 93–100, 2003. View at: Publisher Site | Google Scholar
  10. A. Muan and E. F. Osborn, Phase Equilibria among Oxides in Steel Making, Addison-Wesley, Reading, Mass, USA, 1965.
  11. D. C. Montgomery, Design and Analysis of Experiments, Wiley, New Delhi, India, 5th edition, 2007.
  12. A. Kumar, H. Singh, and S. Maheshwari, “Modeling and analysis by response surface methodology of hardness for submerged arc welded joints using developed agglomerated fluxes,” Indian Journal of Engineering & Materials Sciences, vol. 19, pp. 379–385, 2012. View at: Google Scholar
  13. B. D. Cullity, Elements of X-Ray Diffraction, Addison-Wesley, Reading, Mass, USA, 1978.
  14. P. K. Gordon, “Microstructure of complex ceramics,” in Proceedings of the 3rd Berkeley International Materials Conference, Berkeley, Calif, USA, July 1966. View at: Google Scholar

Copyright © 2013 Ajay Kumar et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.


More related articles

1837 Views | 762 Downloads | 1 Citation
 PDF Download Citation Citation
 Download other formatsMore
 Order printed copiesOrder

Related articles

We are committed to sharing findings related to COVID-19 as quickly as possible. We will be providing unlimited waivers of publication charges for accepted research articles as well as case reports and case series related to COVID-19. Review articles are excluded from this waiver policy. Sign up here as a reviewer to help fast-track new submissions.