Nitridation of niobium oxide films by rapid thermal processing

Anal Bioanal Chem. 2008 Mar;390(6):1507-15. doi: 10.1007/s00216-008-1830-5. Epub 2008 Feb 6.

Abstract

The possibility of forming niobium oxynitride through the nitridation of niobium oxide films in molecular nitrogen by rapid thermal processing (RTP) was investigated. Niobium films 200 and 500 nm thick were deposited via sputtering onto Si(100) wafers covered with a thermally grown SiO(2) layer 100 nm thick. These as-deposited films exhibited distinct texture effects. They were processed in two steps using an RTP system. The as-deposited niobium films were first oxidized under an oxygen atmosphere at 450 degrees C for various periods of time and subsequently nitridated under a nitrogen atmosphere at temperatures ranging from 600 to 1000 degrees C for 1 min. Investigations of the oxidized films showed that samples where the start of niobium pentoxide formation was detected at the surface and the film bulk still consisted of a substoichiometric NbO(x) phase exhibited distinctly lower surface roughness and microcrack densities than samples where complete oxidation of the film to Nb(2)O(5) had occurred. The niobium oxide phases formed at the Nb/substrate interface also showed distinct texture. Zones of niobium oxide phases like NbO and NbO(2), which did not exist in the initial oxidized films, were formed during the nitridation. This is attributed to a "snow-plough effect" produced by the diffusion of nitrogen into the film, which pushes the oxygen deeper into the film bulk. These oxide phases, in particular the NbO(2) zone, act as barriers to the in-diffusion of nitrogen and also inhibit the outdiffusion of oxygen from the SiO(2) substrate layer. Nitridation of the partially oxidized niobium films in molecular nitrogen leads to the formation of various niobium oxide and nitride phases, but no indication of niobium oxynitride formation was found.