Abstract

Nitrogen (and also oxygen) determination has become an important parameter to characterize (oxy)nitride materials for many properties and applications. Analyzing such anions with accuracy is still a challenge for some materials. However, to date, a large panel of methodologies is available to answer this issue with relevant results, even for thin films. Carrier gas hot extraction techniques and electron probe microanalysis with wavelength dispersive spectroscopy (EPMA-WDS) look attractive to analyze bulk materials and thin films, respectively. This paper gathers several techniques using chemical and physical routes to access such anionic contents. Limitations and problems are pointed out for both powders and films.

Highlights

  • In recent decades nitride-type materials have been increasingly studied for diverse applications, for example, in the domains of energy, optics, and the environment [1,2,3,4]

  • (1859–1944)) is a well-known reducing powder composed of 50 wt% aluminum, 45 wt% copper, and

  • Particular attention should be given to the preparation of the samples to remove, as much as possible, the impurities often adsorbed on the surface (CO2, OH, O2, H2 O, N2, NHx, etc.) and, principally, in the case of high specific surface area powders

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Summary

Introduction

In recent decades nitride-type materials have been increasingly studied for diverse applications, for example, in the domains of energy, optics, and the environment [1,2,3,4]. A combination of several methods is necessary to help determine the real contents, as some measurements can be over- or underestimated by the technology and material’s limits. Overlapping between element detection, water contamination, adsorbed species, and high specific surface area powders are examples of situations that can seriously affect the nitrogen/oxygen analyses. This paper reviews some of the techniques to determine the nitrogen content from small (as a dopant in oxides [5,6,7]) to large values (in (oxy)nitrides), as well as oxygen as a co-anion in oxynitride or as an impurity in nitrides. It is important to point out the necessity to obtain standards of high quality to calibrate the measurements. Finding calibration standards with high nitrogen contents (10–20 wt% N). To date only a few papers have raised the issue of nitrogen analyses [8,9,10]

Chemical Methods
Thermogravimetric Analysis
Rietveld Analysis
Kjeldahl Method
Grekov Method
Dumas Method
Combustion Analysis
Physical Methods
Electron Probe Microanalysis
Findings
Conclusions

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