Abstract
Needle-shaped crystals of sizes up to 5 μm × 5 μm × 40 μm of nominal composition KxNbyW1−yO3 were synthesized by solid state method at 800 °C using appropriate amount of WO3, WO2, Nb2O5, and K2WO4. The samples were characterized with XRD, SEM, microprobe analysis, optical spectroscopy, and Raman spectroscopy. The XRD patterns of the samples show single phase of tetragonal tungsten bronze (TTB) type (P4/mbm, No. 127) up to y = 0.07. Structure refinements reveal an increase in cell parameter with increasing nominal niobium content within the TTB phase. The elemental compositions of the crystals determined by electron microprobe analysis also show an increase in Nb content with increasing y. With increasing Nb content the reflectivity minimum in the near infrared spectral range shifts towards lower wavenumber indicating the effect of decreasing carrier concentration. Pyrochlore type phase (KNbWO6) is obtained as a second phase when nominal composition y > 0.07.
Similar content being viewed by others
References
Hägg G (1935) Z Phys Chem B 29:192
Magnéli A (1950) Nova Acta Regiae Soc Sci Upsaliensis 14:4
Magnéli A (1949) Arkiv for Kemi 1:213
Magnali A (1953) Acta Chem Scand 7:315
Hussain A, Kihlborg L (1976) Acta Crystallogr A32:551
Labbe Ph (1992) Key Eng Mater 68:293
Tsuyumoto I, Kudo T (1996) Mat Res Bull 31:17
Granqvist CG (2000) Sol Energ Mater Sol Cells 60:201
Gabel J, Vonau W, Shuk P, Guth U (2004) Solid State Ionics 169:75
Mann M, Shter GE, Reisner GM, Grader GS (2007) J Mater Sci 42:1010. doi:https://doi.org/10.1007/s10853-006-1384-x
Skokan MR, Moulton WG, Morris RC (1979) Phys Rev B 20:3670
Sato M, Grier BH, Shirane G, Fujishita H (1982) Phys Rev B 25:501
Hussain A, Gruehn R, Rüscher CH (1997) J Alloys Compd 246:51
Brusetti R, Haen P, Marcus J (2002) Phys Rev B 65:144528
Brusetti R, Bordet P, Marcus J (2003) J Solid State Chem 172:148
Leitus G, Cohen H, Reich S (2002) Physica C 371:321
Hussain A, Ul-Monir A, Murshed MM, Rüscher CH (2002) Z Anorg Allg Chem 628:416
Debnath T, Rüscher CH, Gesing TM, Koepke J, Hussain A (2008) J Solid State Chem 181:783
Hussain A (1978) Chem Commun Univ Stockholm 2:1
Yang X, Li C, Mo M, Zhan J, Yu W, Yan Y, Qian Y (2003) J Cryst Growth 249:594
Gu Z, Ma Y, Zhai T, Gao B, Yang W, Yao J (2006) Chem Eur J 12:7717
Szilágyi IM, Hange F, Madarász J, Pokol G (2006) Eur J Inorg Chem 17:3413
Szilágyi IM, Madarász J, Pokol G, Király P, Tárkányi G, Saukko S, Mizsei J, Tóth AL, Szabó A, Varga-Josepovits K (2008) Chem Matter 20:4116
Magnéli A (1989) In: 12th European Crystallographic meeting, Moscow
Deschanvres A, Frey M, Raveau B, Thomazea Jc (1968) Bull De La Societe Chim De France:3519
Johansson KE, Palm T, Werner PE (1980) J Phys E: Sci Instrum 13:1289
Werner PE (1970) Arkiv for Kemi 31:513
Raveau B, Thomazea Jc (1968) Comptes Rendus Hebd Des Seances De L Acad Des Sci Serie C 266:540
Miyamoto Y, Kume S, Doumerc JP, Hagenmuller P (1983) Mat Res Bull 18:1463
Dubson MA, Holcomb DF (1985) Phys Rev B 32:1955
Darriet B, Rat M, Galy J (1970) Comptes Rendus Hebd Des Seances De L Acad Des Sci Serie C 271:1324
Feinleib J, Scouler WJ, Ferretti A (1968) Phys Rev B 165:765
Kuhn A, Bashir H, Dos Santos AL, Acosta JL, García-Alvarado F (2004) J Solid State Chem 177:2366
Sanjuán ML, Kuhn A, Azcondo MT, García-Alvarado F (2008) Eur J Inorg Chem 2008:49
Maczka M, Hanuza J, Majchrowski (2001) J Raman Spectrosc 32:929
Acknowledgement
AH is grateful to the Alexander von Humboldt Stiftung, Germany, and University Grants Commission, Bangladesh for financial support. TD thanks the “Land Niedersachsen”, Germany for support with the “Lichtenberg Stipendium” for his Ph.D. research fellowship. Finally, the authors are thankful to two anonymous referees for their helpful comments.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Debnath, T., Roy, S.C., Rüscher, C.H. et al. Synthesis and characterization of niobium-doped potassium tetragonal tungsten bronzes, KxNbyW1−yO3 . J Mater Sci 44, 179–185 (2009). https://doi.org/10.1007/s10853-008-3101-4
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10853-008-3101-4