NH4FeP2O7, NaCaPO4 ve WP2O7 bileşiklerinin mikrodalga enerji yardımıyla sentezlenmesi ve karakterizasyonu

Year 2007, Volume: 9 Issue: 1, 68 - 76, 01.12.2007

Berna Tekin Halil Güler

Abstract

Bu çalışmada, mikrodalga ışınlama yöntemi kullanılarak, tek (Fe, W) ve çift metal (NaCa)
içeren fosfatlı bileşiklerin katı-hal kimyasal reaksiyonları ile sentezlenmesine
çalışılmıştır. Mikrodalga ışınlama kaynağı olarak 2.45 GHz’ lik frekansta çalışan ev
tipi mikrodalga fırın kullanılmıştır. 750 W güç ayarında çalışılmış, reaksiyon süresi 10-
30 dakika arasında tutulmuştur. NH4FeP2O7 bileşiği tek fazlı olarak, NaCaPO4 ve
WP2O7 bileşikleri ise iki fazlı karışımların ana fazları olarak ilk defa mikrodalga
ışınlama yöntemi kullanılarak sentezlenmiştir. Elde edilen ürünler X-ışınları kırınımı
cihazı ve FTIR spektroskopik teknikleri ile karakterize edilmiştir.

Keywords

Mikrodalga ışınlama yöntemi, metal fosfatlar, katı hal kimyası, X- ışınları kırınımı

The synthesis and characterization of NH4FeP2O7, NaCaPO4, WP2O7 compounds using microwave energy

Abstract

In this work, phosphatic compounds containing single (Fe, W) and pair (Na-Ca)metal
were tried to synthesize by using microwave irradition method through solid-state
chemical reactions . As microwave energy source a domestic microwave oven with
frequence of 2,45 GHz were used. The reactions were carried out under power value of
750 W and reaction time was limited with 10-30 minutes. NH4FeP2O7 compound as
single phase, NaCaPO4 and WP2O7 compounds as main phase of mixtures with two
phased were synthesized by using microwave irradition method. The obtained products
were analyzed by XRD (X-Ray diffraction) and FTIR (Fourier Transform IR)
spectroscopic technique..

Keywords

Microwave Đrradition Method, Metal phosphates, Solid-State Chemistry, XRay Diffraction

References

• [1] Hong, H.Y.P., ‘Crystal Structures and Crystal Chemistry in The System Na1+xZr2SixP3-xO12’, Mater. Res. Bull. 11: 173, (1976).
• [2] Moffat, J.B., ‘Phosphates as Catalysts’, Catal. Rev. Sci. Eng. 18: 199, (1978).
• [3] Andrew, Rappe, M., Nicholas, Ramer, J., ‘Quantum Mechanical Đnvestigation of Pyrophosphate Systems’, American Physical Society, March: 12-22, (1996).
• [4] Bennazha, J., Erragh, F., Boukhari, A., Holt, E. M., ‘Đdentification of New Family of Diphosphate Compounds, A2 IB3 II(P2O7)2’, Journal of Chemical Crystallography, 30: 705, (2000).
• [5] Madore, C., Landolt, D., Hassenpflug, C., Herman, J. A., ‘Application of the Rotating Cylinder Hull Cell to the Measurament of Throwing Power and The Monitoring of Copper Plating Baths’, Plating and Surface Finishing, 82(8): 36, (1995).
• [6] Averbuch, M.T. and Durif A.P., ‘Topics in Phosphate in Chemistry’, World Scientific Publication, London, 30 (1996).
• [7] Rao, K.J., Vaidhyanathan, B., Ganguli, M., and Ramakrishnan, P.A., ‘Synthesis of Inorganic Solids Using Microwaves’, Chem. Mater., 11: 882-895, (1999).
• [8] Janney, M.A., Kimrey, H.D., ‘in Ceramic Powder Science II’, Am. Ceram. Soc., 2: 919, (1988).
• [9] Link, G., Ivanov, V., Paranin, S., Khrustov, V., Boehme, R., Müller, G., Schumacher, G., Thumm, M., Weisenburger, A., ‘A Comparison of MM-Wave Sintering and Fast Conventional Sintering of Nanocrystalline Al2O3’, Mater. Res. Soc. Symp. Proc., 430: 157, (1996).
• [10] Meek,T. T., Blake, R. D., Petrovic, J.J., ‘Microwave Sintering of Al2O3±SiC Whisker Composites’, Ceram. Eng. Sci. Proc., 8: 861, (1987).
• [11] Bykov, Y. V., Eremeev, A. G., Holoptsev, V. V., Odemer, C. , Rachkovskii, A. I., Kleissl, H.J.R., ‘Sintering of Piezoceramics Using Millimeter-Wave Radiation’, Ceram. Trans., 80: 321, (1997).