Journal of Thermal Analysis and Calorimetry

, Volume 119, Issue 1, pp 175–182 | Cite as

Thermal stability and structural properties of Ta nanopowder synthesized via simultaneous reduction of Ta2O5 by hydrogen and carbon

  • Loveleen K. Brar
  • Gourav Singla
  • Navjot Kaur
  • O. P. Pandey
Article

Abstract

Tantalum nanoparticles have been synthesized by the single-step chemical reaction route. Simultaneous reduction of Tantalum Pentoxide (Ta2O5) with the in situ produced hydrogen and carbon at 600 °C is a new approach for the production of Ta nanopowder. ΔH values obtained from thermodynamic calculations are used to predict the entire mechanism of reduction of bulk Ta2O5 into Ta nanoparticles. The results of X-ray diffraction studies show that the final product consists of predominately nano α-Ta with β-Ta as the minority phase. The lattice strain in the final product was calculated using Williamson–Hall formula. The effect of lattice strain on thermal stability of the samples was analyzed by differential scanning calorimetry and thermal gravimetry in the air atmosphere. The morphology and particle size distribution of Ta nanosized powders have been analyzed by scanning electron microscope and transmission electron microscope. The results show that average crystallite size of the product Ta nanopowder is about 2–7 nm.

Keywords

Nanoparticles Tantalum α-Ta β-Ta Chemical reaction method 

Notes

Acknowledgements

One of the author (O. P. Pandey) is thankful to Department of Science and Technology (DST), New Delhi, India for which proposal has been submitted. The authors are also grateful to Central Research facilities (IIT Ropar) for providing XRD, IIT Roorkee for providing FE-SEM, SAI Labs, Thapar University for providing SEM and AIIMS, Delhi for providing TEM.

References

  1. 1.
    Won CW, Nersisyan HH, Won HI, Lee JH. Refractory metal nanopowders: synthesis and characterization. Curr Opin Solid State Mater Sci. 2010;14:53–68.CrossRefGoogle Scholar
  2. 2.
    Barnett R, Kilby KT, Fray DJ. Reduction of tantalum pentoxide using graphite and tin-oxide-based anodes via the FFC-Cambridge process. Metall Mater Trans B. 2009;40:150–7.CrossRefGoogle Scholar
  3. 3.
    Wang Y, Cui Z, Zhang Z. Synthesis and phase structure of tantalum nanoparticles. Mater Lett. 2004;58:3017–20.CrossRefGoogle Scholar
  4. 4.
    Xiang H, Xu Y, Zhang L, Cheng L. Synthesis and microstructure of tantalum carbide and carbon composite by liquid precursor route. Scr Mater. 2006;55:339–42.CrossRefGoogle Scholar
  5. 5.
    Zhu H, Sadoway DR. Synthesis of nanoscale particles of Ta and Nb3Al by homogeneous reduction in liquid ammonia. J Mater Res. 2001;16:2544–9.CrossRefGoogle Scholar
  6. 6.
    Othmer K. Encyclopedia of chemical technology. 3rd ed. New York: Wiley; 1978.Google Scholar
  7. 7.
    Kim BS, Choi YY. Kinetics of the chlorination of tantalum pentoxide with carbon tetrachloride gas. Mater Trans, JIM. 2005;46:2102–6.CrossRefGoogle Scholar
  8. 8.
    Yuan B, Okabe TH. Production of fine tantalum powder by preform reduction process using Mg–Ag alloy reductant. J Alloys Compd. 2007;443:71–80.CrossRefGoogle Scholar
  9. 9.
    Wu T, Jin X, Xiao W, Hu X, Wang D, Chen GZ. Thin pellets: fast electrochemical preparation of capacitor tantalum powders. Chem Mater. 2007;19:153–60.CrossRefGoogle Scholar
  10. 10.
    Ayers JD, Anderson IE. Very fine metal powders. JOM. 1985;37:16–21.CrossRefGoogle Scholar
  11. 11.
    Brutvan DR, Ripley RL, Seklemian HV. Ultrafine metal powders. Can Pat. 1965;702:612.Google Scholar
  12. 12.
    Park KY, Kim HJ, Suh YJ. Preparation of tantalum nanopowders through hydrogen reduction of TaCl5 vapor. Powder Technol. 2007;172:144–8.CrossRefGoogle Scholar
  13. 13.
    Awasthi A, Bhatt YJ, Krishnamurthy N, Ueda Y, Garg SP. The reduction of niobium and tantalum pentoxides by silicon in vacuum. J Alloys Compd. 2001;315:187–92.CrossRefGoogle Scholar
  14. 14.
    Baba M, Ono Y, Suzuki RO. Tantalum and niobium powder preparation from their oxides by calciothermic reduction in the molten CaCl2. J Phys Chem Solid. 2005;66:466–70.CrossRefGoogle Scholar
  15. 15.
    De brito RA, Mederios FFP, Gomes UU, Costa FA, Silva AGP, Alves C Jr. Production of tantalum by aluminothermic reduction in plasma reactor. Int J Refract Met Hard Mater. 2008;26:433–7.CrossRefGoogle Scholar
  16. 16.
    Park I, Okabe TH, Lee OY, Lee CR, Waseda Y. Semi-continuous production of tantalum powder by electrochemically mediated reaction (EMR). Mater Trans. 2002;43:2080–6.CrossRefGoogle Scholar
  17. 17.
    Kumar A, Singh K, Pandey OP. Reduction of WO3 to nano-WC by thermo-chemical reaction route. Phys E. 2009;4:677–84.CrossRefGoogle Scholar
  18. 18.
    Singla G, Singh K, Pandey OP. Structural and thermal properties of in situ reduced WO3 to W powder. Powder Technol. 2013;237:9–13.CrossRefGoogle Scholar
  19. 19.
    Demazeau G. Solvothermal reactions: an original route for the synthesis of novel materials. J Mater Sci. 2008;43:2104–14.CrossRefGoogle Scholar
  20. 20.
    Reddy KM, Rao TN, Joardar J. Stability of nanostructured W-C phases during carburization of WO3. Mater Chem Phys. 2011;128:121–6.CrossRefGoogle Scholar
  21. 21.
    Bazhanov DI, Mutigullin IV, Knizhnik AA, Potapkin BV, Bagaturyants AA, Fonseca LRC, Stoker MW. Impact of strain on the surface properties of transition metal carbide films: first-principles study. J Appl Phys. 2010;107:0835211–6.CrossRefGoogle Scholar
  22. 22.
    Read MH, Altman C. A new structure in tantalum thin films. Appl Phys Lett. 1965;7:51–2.CrossRefGoogle Scholar
  23. 23.
    Díez VK, Apesteguía CR, Di Cosimo JI. Effect of the acid-base properties of Mg–Al mixed oxides on the catalysts deactivation during aldol condensation reactions. Lat Am Appl Res. 2003;33:79–86.Google Scholar
  24. 24.
    Kamberović Ž, Filipović D, Raić K, Tasić M, Anđić Z, Gavrilovski M. Reduction of ultra-fine tungsten powder with tungsten (VI) oxide in a vertical tube reactor. Mater Technol. 2011;45:27–32.Google Scholar
  25. 25.
    Dabhade VV, Mohan TRR, Ramakrishnan P. Nanocrystalline titanium powders by high energy attrition milling. Powder Technol. 2007;171:177–83.CrossRefGoogle Scholar
  26. 26.
    Cheng HKF, Chong MF, Liu E, Zhou K, Li L. Thermal decomposition kinetics of multiwalled carbon nanotube/polypropylene nanocomposites. J Therm Anal Calorim. 2014;117:63–71.CrossRefGoogle Scholar
  27. 27.
    Díaz-Ayala R, Arroyo-Ramírez L, Raptis RG, Cabrera CR. Thermal and surface analysis of palladium pyrazolates molecular precursors. J Therm Anal Calorim. 2014;115:479–88.CrossRefGoogle Scholar
  28. 28.
    Haines PJ. Principles of thermal analysis and calorimetry. Cambridge: Royal Society of Chemistry; 2002.CrossRefGoogle Scholar
  29. 29.
    Brown ME. Handbook of thermal analysis and calorimetry. 1st ed. New york: Elsevier Science; 1998.Google Scholar
  30. 30.
    Yoon JS, Park HH, Bae IS, Goto S, Kim BI. Production of tantalum powder by external continuous supply of feed materials and reductant. Mater Trans. 2005;46:272–6.CrossRefGoogle Scholar
  31. 31.
    Debalina B, Kamaraj M, Chakravarthi SR, Vasa NJ, Sarathi R. Understanding the mechanism of nanoparticle formation in a wire explosion process by adopting the optical emission technique. Plasma Sci Technol. 2013;15:562–9.CrossRefGoogle Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2014

Authors and Affiliations

  • Loveleen K. Brar
    • 1
  • Gourav Singla
    • 1
  • Navjot Kaur
    • 1
  • O. P. Pandey
    • 1
  1. 1.School of Physics and Materials ScienceThapar UniversityPatialaIndia

Personalised recommendations