A method of determining nanoparticle size distribution in iron ammonia synthesis catalyst by measuring mass changes during the nitriding process

•Method for determining the nanoparticle size distribution in catalysts is proposed.•Fused iron catalyst for ammonia synthesis was used.•Kinetics of nanocrystalline iron nitriding with ammonia was studied.•Nanocrystallite size distribution by the new method was verified by other methods.•The new method has a great practical implications in characterization of catalysts.

A new method for determination of nanoparticle size distribution, on the basis of measurements of nanomaterial conversion degree as a function of the chemical potential of gas reagent, was presented. The method was applied for determination of nanocrystallite size distribution in a pre-reduced iron catalyst for ammonia synthesis being an example of a nanomaterial. Samples were reduced with hydrogen at 500 °C and then nitrided at 300 °C in gaseous ammonia-hydrogen mixtures of different nitriding potentials. Conversion degree measurements, viz., measurements of mass changes of the catalyst were performed in a differential reactor equipped with systems that enable thermogravimetric measurements and analysis of gas phase chemical composition. Based on the performed measurements, a relationship binding the conversion degree with size distribution was proposed. The resulting size distribution of nanocrystallites was compared to distributions determined by known techniques based on XRD or on measurements of the nitriding reaction rate. The size distribution determined using the new method has a higher resolution, revealing more details of the sample morphology.

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