Journal of Materials Science

, Volume 44, Issue 16, pp 4252–4257 | Cite as

Energy-efficient green synthesis of Nd:Y2O3 nanopowder by microwave gel combustion

  • Mann RekhaEmail author
  • Kiranmala Laishram
  • Ravi Kumar Gupta
  • Neelam Malhan
  • Ashok Kumar Satsangi


A novel method for the synthesis of nanocrystalline neodymium-doped yttria (Nd:Y2O3) by gel combustion in microwave without long period of calcination at high temperature is described. The method leads to rapid formation of phase pure product with saving of time and energy. Gels were prepared by selecting citrate to nitrate (C/N) ratios of 0.5:1 & 1:1 followed by combustion in microwave for drying of gel leading to precursor formation. Thermogravimetric-differential thermal analysis (TG-DTA) of precursor with (C/N) ratios of 1:1 exhibited a total loss in weight of about 31.7% up to 1300 °C and did not show M–O bonds characteristic of yttria by FTIR indicating requirement of calcination at high temperature. Crystallization to phase pure yttria took place only on thermal treatment at 1000 °C for 4 h in oxygen atmosphere confirmed by XRD with particle size 40 nm. While the microwave combusted precursor with C/N ratio of 0.5:1 exhibited a weight loss of only 4.7% up to 1300 °C and showed M–O bonds characteristic of yttria in FTIR spectrum without calcinations at higher temperature. This microwave combustion precursor with C/N ratio of 0.5:1 was found to be crystalline phase pure yttria by X-ray diffraction (XRD) with primary particle size 28 nm by Scherrer’s equation and 30–50 nm of uniform morphology by transmission electron microscopy (TEM). In the present work the ratio of citric acid to nitrates is playing a crucial role in terms of saving time and energy involved in calcinations of microwave combusted precursor for the composition with higher citrate content.


Calcination Y2O3 Primary Particle Size Yttrium Nitrate Citric Acid Anhydrous 



We would like to thank Director, Laser Science and Technology Centre, Defence Research and Development Organization (DRDO), Delhi, for the encouragement and support to carry out this work. Further we extend our thanks to Dr. Prasoon Roy, Scientist ‘D’, Centre for Fire, Explosive and Environment, and Mr. Anshu, Scientist ‘B’, Solid State Physics Laboratory, DRDO, Delhi, for their timely help during various characterizations.


  1. 1.
    Fokema MD, Chiu E, Ying JY (2000) Langmuir 16(7):3154CrossRefGoogle Scholar
  2. 2.
    Tomaszewski H, Weglarz H, De Gryse R (1997) J Eur Ceram Soc 17:403CrossRefGoogle Scholar
  3. 3.
    Akinc M, Celikkaya A (1987) Advances in ceramics. Inc. Press, Westerville, OHGoogle Scholar
  4. 4.
    Rulison AJ, Flagan RC (1994) J Am Ceram Soc 77:3244CrossRefGoogle Scholar
  5. 5.
    Dupont A, Parent C, Garrecand BL, Heintz JM (2003) J Solid State Chem 171(1–2):152CrossRefGoogle Scholar
  6. 6.
    Mouzon J, Odén M (2007) Powder Tech 177(2):77CrossRefGoogle Scholar
  7. 7.
    Ekambaram S, Patil KC (1995) J Mater Chem 5:905CrossRefGoogle Scholar
  8. 8.
    Kakade B, Ramanathan S, Ravindran PV (2003) J Alloys Compd 350(1–2):123CrossRefGoogle Scholar
  9. 9.
    Rahamana MN (2003) Ceramic processing and sintering, 2nd edn. CRC Press, LondonGoogle Scholar
  10. 10.
    Bondioli F, Ferrari AM, Leonelli C, Siligardi C et al (2001) J Mater Chem 11:2620CrossRefGoogle Scholar
  11. 11.
    Nyutu EK, Chen CH, Sithambaram S et al (2008) J Phys Chem C 112(17):6786CrossRefGoogle Scholar
  12. 12.
    Manglaraja RV, Ramam KVS et al (2007) Mater Sci Pol 25(4):1075Google Scholar
  13. 13.
    Panneer SM, Subanna GN, Rao KJ (2001) J Mater Res 16(10):2773CrossRefGoogle Scholar
  14. 14.
    Subramanian V, Burke WW, Zhu H, Wei B (2008) J Phys Chem C 112(12):4550CrossRefGoogle Scholar
  15. 15.
    Vishnuvardhan TK, Kulkarni VR, Basavaraja C, Raghavendra SC (2006) Bull Mater Sci 29(1):77CrossRefGoogle Scholar
  16. 16.
    da Vila LD, Stucchi EB, Davolos MR (1997) J Mater Chem 7(10):2113CrossRefGoogle Scholar
  17. 17.
    Culity BD, Stock SR (1978) Elements of X-ray diffraction. Addison, Wesley, MAGoogle Scholar
  18. 18.
    Bartos A et al (1993) Acta Crystallogr B Struct Sci 49:165CrossRefGoogle Scholar
  19. 19.
    Kaygorodov AS, Ivanov VV et al (2007) J Eur Ceram Soc 27(2–3):1165CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2009

Authors and Affiliations

  • Mann Rekha
    • 1
    Email author
  • Kiranmala Laishram
    • 1
  • Ravi Kumar Gupta
    • 2
  • Neelam Malhan
    • 1
  • Ashok Kumar Satsangi
    • 1
  1. 1.Chemistry Division, Laser Science and Technology CentreDRDODelhiIndia
  2. 2.Directorate of Public InterfaceDRDO Headquarters, DRDO BhawanDelhiIndia

Personalised recommendations