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Mechanism on reduction and nitridation of micrometer‐sized titania with ammonia gas
Author(s) -
Liu Yongjie,
Wang Yue,
Zhang Yu,
You Zhixiong,
Lv Xuewei
Publication year - 2020
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/jace.17067
Subject(s) - tin , anatase , titanium nitride , x ray photoelectron spectroscopy , oxygen , stoichiometry , nitrogen , ammonia , inorganic chemistry , titanium , nitride , materials science , chemistry , analytical chemistry (journal) , chemical engineering , metallurgy , catalysis , nanotechnology , photocatalysis , organic chemistry , engineering , layer (electronics)
Ammonia gas can be simultaneously used as a reductant and nitrogen source to prepare TiN from titania. In this work, the mechanisms on reduction and nitridation of micrometer‐sized anatase with ammonia gas have been investigated, using both thermodynamic and experimental studies. The thermodynamic analysis indicated that reduction and nitridation of TiO 2 by NH 3 was feasible. Anatase will undergo different paths to form TiN, depending on the reaction temperature. Upon heating, NH 3 was seen to partially decompose into N 2 and H 2 , although the actual NH 3 decomposition ratio was less than the theoretical value. The experimental results indicated that the obtained titanium nitride was non‐stoichiometric (TiN x O 1 −x , x  ≤ 1), as it contained a certain amount of oxygen. Based on the phase transformation and X‐ray photoelectron spectroscopy analysis, the reduction and nitridation routes were deduced: TiO 2 reacted with NH 3 to form TiN x O 1− x directly, at lower temperatures, and followed the path TiO 2  → Ti n O 2n−1  → TiN x O 1− x , at higher temperatures. Ti n O 2n−1 was determined to be Ti 4 O 7 and Ti 3 O 5 at 1100°C and 1200°C, respectively. Reaction temperature and time significantly affected the oxygen and nitrogen contents in TiN x O 1− x , with the lattice parameter of roasted products gradually increasing—approaching those of pure TiN—with an increase in reaction temperature and holding time. At the same time, the content of oxygen in TiN x O 1− x decreased, and its nitrogen content correspondingly increased.

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