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2 Journal of Achievements in Materials and Manufacturing Engineering

2 2014

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Microwave synthesis and characterization of non-stoichiometric Mg0.1551Fe1.8966O3

Celik G., Somunkiranoglu S., Kurtulus F.

Journal of Achievements in Materials and Manufacturing Engineering

2014

Vol. 65, nr 1

5--9

Purpose: of this study is clearly different synthesis method (microwave method) of non-stoichiometric magnesium iron oxide using in broad area such as high frequency magnets, data storage systems and especially cancer treatment. Design/methodology/approach: Analytically magnesium oxide and iron (III) oxide weighed an appropriate molar ratio and homogenized in an agate mortar. The mixture placed into a porcelain crucible to heat in microwave oven. After the material was exposed to microwave irritation, it was taken from the oven, and then homogenized again. Then, final product was ready to analyse. Powder X-ray Diffractometer (XRD) was used to determine crystal structure of the product. FTIR spectrum was taken to support the functional groups. Thermo gravimetric-differential thermal analysis (TG/DTA) was carried out to identify thermal character. Morphological properties and semi-quantitative analyse of the sample was performed by Scanning electron microscope/ Electron disperse (SEM/EDX). Findings: The XRD patterns show that the product is Mg0.1551Fe1.8966O3 (ICSD 51171). The first time synthesized material is crystallized in hexagonal system with unit cell parameters a=5.0490, b=5.0490, c=13.7890 Å and space group R-3c. The other supporting methods confirm the crystal structure. Non-stoichiometric Mg0.1551Fe1.8966O3 (ICSD 51171) was synthesized by microwave method completely different from literature for the first time. The characterization was mainly based on powder X-ray diffraction pattern. Also, thermal behaviour and morphology were determined. Research limitations/implications: The synthesis method has some disadvantages such as low repeatability, non-uniform product etc. We tried to minimize these negative aspects in our research and succeeded. Practical implications: The compound can be used to reduce side-effects of drugs for cancer treatment, and find broad usage area in that treatment. For his reason, magnesium iron oxide has practical applications. Originality/value: The originality of the paper is first time microwave synthesis of Mg0.1551Fe1.8966O3. In the literature, the magnesium iron oxide was synthesized so many times by different conventional routes. But, as far as we know cheap, clean and short-term synthesis route has not been used before.

Hydrothermal synthesis and characterization of double phase magnesium vanadium oxides

Celik G., Somunkiranoglu S., Kurtulus F.

Journal of Achievements in Materials and Manufacturing Engineering

2014

Vol. 63, nr 2

53--57

Purpose: The electronic conductivity of derivatives of MgxVyOz type compounds is magnitude higher than that of the vanadium oxide without magnesium. Also, magnesium containing compounds exhibit significantly improved kinetic behaviour and rate capability. In this perspective, we aim to synthesis of magnesium vanadium oxide under mild hydrothermal conditions. Design/methodology/approach: Double phase magnesium vanadium oxides were synthesized by dissolving magnesium nitrate and V2O5 in the ultra pure water with in an appropriate molar ratio. The homogeneous solution in the stainless-steel container was put into furnace and heated 3 days (72 hours) at 180ºC. The product was washed by high pure water and ethanol, dried at 70ºC for 2 hours and homogenized in an agate mortar. Then, final product was ready to analyse. Powder X-ray Diffractometer (XRD) was used to determine crystal structure of the product. FTIR spectrum was taken to support the functional groups. Thermo gravimetric-differential thermal analysis (TG/DTA) was carried out to identify thermal character. Morphological properties and semi-quantitative analyse of the sample was performed by Scanning electron microscope/Electron disperse (SEM/EDX). Phase analyse was realized by High Score Plus Program. Findings:The XRD patterns show that the product is Mg0.01V2O5 (ICDD:89-0610)-β-Mg1.9V3O8 (ICDD:23-1232). The result of phase analyse show that the sample contains %27.2 Mg0.01V2O5 and %72.8 β-Mg1.9V3O8. The mixture was obtained under mild hydrothermal conditions for the first time as distinct from literature. Characterization studies were mainly based on powder X-ray diffraction technique. Also, thermal behaviour, morphology and percentage of component were determined. Research limitations/implications:The principal of hydrothermal method is low temperature/high pressure synthesis in water. Sometimes, optimizing of the most convenient condition can be time and chemical consuming. This situation could be a limit to use hydrothermal method. But, this can eliminate with deep background. Practical implications: The compounds can find many application areas utilizing kinetic behaviour, rate capability and electronic conductivity properties. Originality/value: We achieved the hydrothermal synthesis of Mg0.01V2O5 (ICDD:89-0610)- β-Mg1.9V3O8 (ICDD:23-1232) under mild hydrothermal conditions for the first time as distinct from literature.