Abstract

Palladium doped anatase TiO2 nanoparticles were synthesised by a rapid (3 min) one-pot microwave synthesis technique at low temperature and pressure. After being fully characterised by SEM, XRD, Raman, XPS and EDX, photocatalytic nitrate reduction and ammonia production were studied over various dopant levels between 0–3.97 wt% Pd and compared to similar previous literature. Improved yields of ammonia were observed with most dopant levels when compared to non-doped microwave synthesised TiO2 with 2.65 wt% found to be the optimum dopant level producing 21.2 μmol NH3. Electrochemical impedance spectroscopy of TiO2 and Pd–TiO2 photoelectrodes revealed improvements in charge transfer characteristics at high Pd dopant levels.

Highlights

  • Ammonia (NH3) is the most produced commercial chemical in the world with its production ever increasing, as in 2012 it was up to 160 million tons per annum.[1]

  • We investigate the photocatalytic nitrate reduction properties microwave synthesised TiO2 and various dopant levels of Pd–TiO2 in comparison to previously reported literature methods of similar photocatalysts with conventional synthesis techniques

  • SEM studies show the formation of nanoparticles made via microwave synthesis

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Summary

Introduction

Ammonia (NH3) is the most produced commercial chemical in the world with its production ever increasing, as in 2012 it was up to 160 million tons per annum.[1] Its signi cant use is in the fertilizer industry where over-manuring has caused a signi cant increase of the concentration of harmful nitrate ions (NO3À) in groundwater.[2] Nitrate ions and their derivatives are considered water pollutants as toxic levels have been shown to cause methemoglobinemia in infant children and act as a possible promotor of carcinogenesis.[3,4] Release of nitrate into groundwater is well-known to cause eutrophication destroying ecosystems with higher levels of nitrate This has led to considerable research into nitrate reduction via a range of different techniques including biological,[5] electrochemical,[6,7,8] and catalytic methods.[9,10,11] Among these methods photocatalytic reduction stands out as a sustainable, potentially scalable and environmentally friendly solution with the ability to reduce aqueous nitrate to nitrogen or ammonia utilising only a suitable photocatalyst, water and sunlight. These ndings are important in the context of current efforts to nd a more sustainable means of sustainable ammonia production as well as reduction of nitrates in wastewater

Microwave synthesis of Pd–TiO2
Characterisation of Pd–TiO2 photocatalyst
Photocatalytic studies
Ammonia detection
Electrochemical studies
SEM analysis
XRD analysis
Raman analysis
XPS analysis
EDX analysis
Photocatalytic activity
Electrochemical analysis
Conclusions

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