TY - JOUR
T1 - Accessing the rich carbon nitride materials chemistry by heat treatments of ammonium thiocyanate, NH 4 SCN
AU - Larsen, Finn Krebs
AU - Hasen Mamakhel, Aref
AU - Overgaard, Jacob
AU - Jørgensen, Jens Erik
AU - Kato, Kenichi
AU - Brummerstedt Iversen, Bo
PY - 2019/8
Y1 - 2019/8
N2 - Carbon nitride materials include functional materials, and their chemical diversity and complexity are becoming increasingly appreciated. Heating of NH 4 SCN leads to a range of new carbon nitride compounds, which have been structurally characterized by single-crystal X-ray diffraction. Heating at ambient pressure to 175°C leads to guanidinium thiocyanate, H 6 CN 3 SCN (1), and when maintaining that temperature for about 12h a water-insoluble carbon nitride product is formed, which is a co-crystal between melamine and melamium thiocyanate, [H 6 C 3 N 6 ]·[H 10 C 6 N 11 ] + ·[SCN] - (2). In situ powder X-ray diffraction measurements of this material reveal a gradual transformation from (2), via two intermediate products, to a final melon-like end product. The first of these forms between 350 and 400°C, and is an adduct of melam and melamium thiocyanate, [H 9 C 6 N 11 ]·2[H 10 C 6 N 11 ] + ·2[SCN] - (3). The second forms between 400 and 480°C, and is identified as melem, 2,5,8-triamino-tri-s-triazine, H 6 C 6 N 10 (4). On heating of (2) in a sealed ampoule to 600°C, various crystals were obtained and six crystal structures were determined from the batch: 1,3,5-triazine-2,4,6-triamino, H 6 C 3 N 6 (5), 1,3,5-triazine-2,4-diamino, H 5 C 3 N 5 (6), 1,1′,3,3′,5,5′-triazine-2,2′,4,4′-tetraamino, H 8 C 6 N 10 (7), 2[H 6 C 3 N 6 ]·[H 10 C 6 N 11 ] + ·[SCN] - (8) and 2[H 6 C 3 N 6 ]·[H 7 C 3 N 6 ] + ·[SCN] - (9). Finally, a recrystallized decomposition product was found to be [H 6 C 3 N 6 ]·[H 7 C 3 N 6 ] + ·[SCN] - ·[H 2 O] (10).
AB - Carbon nitride materials include functional materials, and their chemical diversity and complexity are becoming increasingly appreciated. Heating of NH 4 SCN leads to a range of new carbon nitride compounds, which have been structurally characterized by single-crystal X-ray diffraction. Heating at ambient pressure to 175°C leads to guanidinium thiocyanate, H 6 CN 3 SCN (1), and when maintaining that temperature for about 12h a water-insoluble carbon nitride product is formed, which is a co-crystal between melamine and melamium thiocyanate, [H 6 C 3 N 6 ]·[H 10 C 6 N 11 ] + ·[SCN] - (2). In situ powder X-ray diffraction measurements of this material reveal a gradual transformation from (2), via two intermediate products, to a final melon-like end product. The first of these forms between 350 and 400°C, and is an adduct of melam and melamium thiocyanate, [H 9 C 6 N 11 ]·2[H 10 C 6 N 11 ] + ·2[SCN] - (3). The second forms between 400 and 480°C, and is identified as melem, 2,5,8-triamino-tri-s-triazine, H 6 C 6 N 10 (4). On heating of (2) in a sealed ampoule to 600°C, various crystals were obtained and six crystal structures were determined from the batch: 1,3,5-triazine-2,4,6-triamino, H 6 C 3 N 6 (5), 1,3,5-triazine-2,4-diamino, H 5 C 3 N 5 (6), 1,1′,3,3′,5,5′-triazine-2,2′,4,4′-tetraamino, H 8 C 6 N 10 (7), 2[H 6 C 3 N 6 ]·[H 10 C 6 N 11 ] + ·[SCN] - (8) and 2[H 6 C 3 N 6 ]·[H 7 C 3 N 6 ] + ·[SCN] - (9). Finally, a recrystallized decomposition product was found to be [H 6 C 3 N 6 ]·[H 7 C 3 N 6 ] + ·[SCN] - ·[H 2 O] (10).
KW - 2D materials
KW - ammonium thiocyanate decomposition
KW - carbon nitride compounds
KW - crystal structure
UR - http://www.scopus.com/inward/record.url?scp=85068266697&partnerID=8YFLogxK
U2 - 10.1107/S2052520619005791
DO - 10.1107/S2052520619005791
M3 - Journal article
C2 - 32830719
AN - SCOPUS:85068266697
SN - 2052-5192
VL - 75
SP - 621
EP - 633
JO - Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
JF - Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
ER -