Synthesis of titanium nitride via hybrid nanocomposites based on mesoporous TiO2/acrylonitrile

Claudiu Locovei,Andrei Sârbu,Andreea Miron,Anita-Laura Chiriac,Anca Dumitru,Sorina Iftimie,Vlad-Andrei Antohe

doi:10.1038/s41598-021-84484-3

Abstract

In the present study, the synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored. The choice of hybrid nanocomposite as precursor for the synthesis of TiN was made due to the possibility of having an intimate interface between the organic and inorganic phases in the mixture that can favours CRN reaction. Subsequently, the hybrid composites have been subjected to four-step thermal treatments at 290 °C, 550 °C, 1000 °C and 1400 °C under nitrogen atmosphere. The XRD results after thermal treatment at 1000 °C under nitrogen flow show the coexistence of two crystalline phases of TiO2, i.e. anatase and rutile, as well as TiN phase, together with the detection of amorphous carbon that proved the initiation of CRN reaction. Furthermore, the observations based on XRD patterns of samples thermally treated at 1400 °C in nitrogen atmosphere were in agreement with SEM analysis, that shows the formation of TiN by CRN reaction via hybrid nanocomposites mesoporous TiO2/acrylonitrile.

Highlights

In the present study, the synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored
Hybrid nanocomposite based on mesoporous T iO2/acrylonitrile monomers with different content of inorganic phase, were explored for the synthesis of TiN by CRN reaction
The structural analysis based on XRD analysis of the samples thermal treated at 1400 °C in nitrogen atmosphere highlighted the formation of crystalline TiN phase as main phase along with some traces of impurities in the form of amorphous graphite and amorphous graphite oxide

Summary

Introduction

The synthesis of titanium nitride (TiN) by carbothermal reduction nitridation (CRN) reaction using nanocomposites made of mesoporous TiO2/acrylonitrile with different content of inorganic phase were explored. Despite the relatively low temperatures range used for TiN synthesis, these methods still have some limitations, mostly related either to the expensive ionic liquids required, or to the extremely poisonous and dangerous reactants used as nitrogen source[1]. In this regard, the development of economical and environmentally friendly preparation route of TiN is highly desirable. Hybrid nanocomposite materials were obtained by radical polymerization of a vinyl monomer in pre-synthesized mesoporous T iO2 and further used as starting materials for the synthesis of TiN by CRN reaction at 1400 °C under nitrogen gas flow

Methods

Results

Conclusion