Bulletin of Materials Science

, Volume 26, Issue 4, pp 449–460 | Cite as

Thermogravimetry-evolved gas analysis-mass spectrometry system for materials research

  • M Kamruddin
  • P K Ajikumar
  • S Dash
  • A K Tyagi
  • Baldev Raj
Article
Received:

Abstract

Thermal analysis is a widely used analytical technique for materials research. However, thermal analysis with simultaneous evolved gas analysis describes the thermal event more precisely and completely. Among various gas analytical techniques, mass spectrometry has many advantages. Hence, an ultra high vacuum (UHV) compatible mass spectrometry based evolved gas analysis (EGA-MS) system has been developed. This system consists of a measurement chamber housing a mass spectrometer, spinning rotor gauge and vacuum gauges coupled to a high vacuum, high temperature reaction chamber. A commercial thermogravimetric analyser (TGA: TG + DTA) is interfaced to it. Additional mass flow based gas/vapour delivery system and calibration gas inlets have been added to make it a versatile TGA-EGA-MS facility. This system which gives complete information on weight change, heat change, nature and content of evolved gases is being used for (i) temperature programmed decomposition (TPD), (ii) synthesis of nanocrystalline materials, (iii) gas-solid interactions and (iv) analysis of gas mixtures. The TPD of various inorganic oxyanion solids are studied and reaction intermediates/products are analysed off-line. The dynamic operating conditions are found to yield nanocrystalline products in many cases. This paper essentially describes design features involved in coupling the existing EGA-MS system to TGA, associated fluid handling systems, the system calibration procedures and results on temperature programmed decomposition. In addition, synthesis of a few nanocrystalline oxides by vacuum thermal decomposition, gas analysis and potential use of this facility as controlled atmosphere exposure facility for studying gas-solid interactions are also described.

Keywords

Evolved gas analysis thermogravimetry mass spectrometry temperature programmed decomposition gas-solid interaction nano-materials 
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References

  1. Akermark Torbjorn 1998Oxid. Met. 50 167CrossRefGoogle Scholar
  2. Alok Singh, Dash S, Kamruddin M, Ajikumar P K, Tyagi A K, Raghunathan V S and Baldev Raj 2002J. Am. Ceram. Soc. 85 927Google Scholar
  3. Barnes P A 1987Thermochim. Acta 114 1CrossRefGoogle Scholar
  4. Brown Micheal E 1998Handbook of thermal analysis, Principles and practice (New York: Elsevier)Vol. 1, p. 509Google Scholar
  5. Charsley E L, Manning N J and Warrington S B 1987Thermochim. Acta 114 47CrossRefGoogle Scholar
  6. Dash S, Kamruddin M and Tyagi A K 1997aBull. Mater. Sci. 20 359Google Scholar
  7. Dash S, Krishnan R, Rajagopalan S and Tyagi A K 1997bProc. int. conf. corrosion and its control (CONCORN97), Mumbai (eds) A S Khannaet al (Amsterdam: Elsevier) p. 939Google Scholar
  8. Dash S, Krishnan R, Paulraj M, Balamurugan A K, Rajagopalan S, Kamruddin M and Tyagi A K 1997cProc. symp. localized corrosion and environmental cracking (Kalpakkam:IGCAR) (compiled by H S Khatak and S Rajendran Pillai), p. C-30Google Scholar
  9. Dash S, Kamruddin M, Ajikumar P K, Krishnan R and Tyagi A K 1998Indian J. Chem. Technol. 5 35Google Scholar
  10. Dash S, Ajikumar P K, Kamruddin M and Tyagi A K 1999aThermochim. Acta 334 141CrossRefGoogle Scholar
  11. Dash S, Kamruddin M, Santanu Bera, Ajikumar P K, Tyagi A K, Narasimhan S V and Baldev Raj 1999bJ. Nucl. Mater. 264 271CrossRefGoogle Scholar
  12. Dash S, Kamruddin M, Ajikumar P K, Tyagi A K, Baldev Raj, Santanu Bera and Narasimhan S V 2000aJ. Nucl. Mater. 278 173CrossRefGoogle Scholar
  13. Dash S, Kamruddin M, Ajikumar P K, Tyagi A K and Baldev Raj 2000bThermochim. Acta 363 129CrossRefGoogle Scholar
  14. Dash S, Krishnan R, Kamruddin M, Tyagi A K and Baldev Raj 2001J. Nucl. Mater. 295 281CrossRefGoogle Scholar
  15. Dash S, Alok Singh, Ajikumar P K, Subramanian H, Rajalakshmi M, Tyagi A K, Arora A K, Narasimhan S V and Baldev Raj 2002J. Nucl. Mater. 303 156CrossRefGoogle Scholar
  16. Dollimore D, Gamlen G A and Taylor T J 1984Thermochim. Acta 75 59CrossRefGoogle Scholar
  17. Franchy R 2000Surf. Sci. Rep. 38 195CrossRefGoogle Scholar
  18. Fremory J K and Boden K 1978J. Phys. E11 106Google Scholar
  19. Gadalla A M 1985Thermochim. Acta 95 179CrossRefGoogle Scholar
  20. Gallagher P K 1982J. Thermal Anal. 25 7CrossRefGoogle Scholar
  21. Gorte R J 1996Catal. Today 28 405CrossRefGoogle Scholar
  22. Heide K, Gerth K, Buchel G and Hartmann E 1997J. Thermal Anal. 48 73CrossRefGoogle Scholar
  23. Heide K, Hartmann E, Gert K and Wiedemann H G 2000Thermochim. Acta 365 147CrossRefGoogle Scholar
  24. Janakiraman R, Meier G and Pettit F S 1999Metall. Mater. Trans. A30 2905CrossRefGoogle Scholar
  25. Jedlinski J and Borchardt G 1991Oxid. Met. 36 317CrossRefGoogle Scholar
  26. Jemal M and Khattech I 1989Thermochim. Acta 152 65CrossRefGoogle Scholar
  27. Kaisersberger E and Post E 1997Thermochim. Acta 295 73CrossRefGoogle Scholar
  28. Kamruddin M, Ajikumar P K, Dash S, Purniah B, Tyagi A K and Krishan K 1995Instrum. Sci. Technol. 23 123CrossRefGoogle Scholar
  29. Kamruddin M, Ajikumar P K, Dash S, Krishnan R, Tyagi A K and Krishan K 1996Thermochim. Acta 287 13CrossRefGoogle Scholar
  30. Kamruddin M, Ajikumar P K, Dash S, Krishnan R, Tyagi A K and Krishan K 1997J. Thermal Anal. 48 277CrossRefGoogle Scholar
  31. Kamruddin M, Shemet V, Singheisiser L, Tyagi A K and Quadakkers W J 2000Proc. of international symp. on materials aging and life management, Kalpakkam (New Delhi: Allied Publishers Limited) p. 815Google Scholar
  32. Kamruddin M, Ajikumar P K and Tyagi A K 2001Workshop on complete cycle characterization of materials, Kalpakkam Google Scholar
  33. Kamruddin M, Ajikumar P K, Dash S and Tyagi A K 2002IGCAR News Letter 51 7Google Scholar
  34. Leskela T, Lippmaa M, Niinisto L and Soininen P 1993Thermochim. Acta 214 9CrossRefGoogle Scholar
  35. Maciejewski M and Baiker A 1997Thermochim. Acta 295 95CrossRefGoogle Scholar
  36. Medeiros F F P, De Oliveria S A, De Souza C P, Da Silva AGP, Gomes U U and De Souza J F 2001Mater. Sci. & Eng. A315 58CrossRefGoogle Scholar
  37. Mullens J, Carleer R, Reggers G, Yperman J, Vanhees J and Van Poucke L C 1992Thermochim. Acta 212 219CrossRefGoogle Scholar
  38. Mullens J, Reggers G, Rusen M, Carleer R,Yperman J, Vanhees J, Franko D and Van Poucke L C 1997J. Thermal Anal. 49 1061CrossRefGoogle Scholar
  39. Nielsen M, Jurasek P, Hayashi J and Furimsky E J 1995Anal. Appl. Pyrol. 35 43CrossRefGoogle Scholar
  40. Ohrbach Karl-Heinz, Radhoff Gabriele and Kettrup Antonius 1983Thermochim. Acta 67 189CrossRefGoogle Scholar
  41. Ozawa Takeo 2000Thermochim. Acta 352–353 177CrossRefGoogle Scholar
  42. Price D, Dollimore D, Fatemi N S and Whitehead R 1980Thermochim. Acta 42 323CrossRefGoogle Scholar
  43. Raemaekers K G H and Bart J C J 1997Thermochim. Acta 295 1CrossRefGoogle Scholar
  44. Remmler M, Kopinke F-D and Stottmeister U 1995Thermochim. Acta 263 101CrossRefGoogle Scholar
  45. Statheropoulos M and Kyriakou S A 2000Anal. Chim. Acta 409 203CrossRefGoogle Scholar
  46. Suryanarayana C and Norton M G 1998X-ray diffraction: A practical approach (New York: Plenum) p. 207Google Scholar
  47. Waime H, Centeno M A, Picard S, Bastians P and Grange P 1998J. Eur. Ceram. Soc. 18 1293CrossRefGoogle Scholar

Copyright information

© Indian Academy of Sciences 2003

Authors and Affiliations

  • M Kamruddin
    • 1
  • P K Ajikumar
    • 1
  • S Dash
    • 1
  • A K Tyagi
    • 1
  • Baldev Raj
    • 1
  1. 1.Metallurgy and Materials GroupIndira Gandhi Centre for Atomic ResearchKalpakkamIndia

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