Chemical species in sulfur-ammonia solutions: influence of amide addition

Dubois, Philippe; Lelieur, J. P.; Lepoutre, G.

doi:10.1021/ic00290a027

Cited by 25 publications

(16 citation statements)

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“…S dissolved ) was also validated through UV-vis spectroscopy. The absorbance bands at 232, 360 and 305 nm in the UV-vis spectra may be respectively assigned to HS − , S 2− ions [37,38] and zero-oxidation sulfur (S 0 ) in soluble state [36,39]. The band at 232 nm can be ascribed to S 2 O 2− 3 ions.…”

Section: Hsmentioning

confidence: 96%

Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Panigrahi¹,

Pathak²

2008

Science and Technology of Advanced Materials

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Tungsten disulfide (WS 2 ) nanowires have been synthesized through a microwave-assisted chemical route that uses tungstic acid, elemental sulfur and monoethanolamine as starting reagents for obtaining a precursor solution of tetrathiotungstate ions. Acidification of the precursor solution yields amorphous precipitates, which lead to the formation of nanowires of WS 2 with thickness of about 5-10 nm when heated at 750• C under argon atmosphere for 1.5 h. Phase and the microstructure of the prepared powders have been investigated through x-ray powder diffraction and high-resolution transmission electron microscopy, respectively. Optical absorption of the WS 2 powders reveals a red shift of the exciton bands compared to bulk WS 2 .

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Section: Hsmentioning

confidence: 96%

Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Panigrahi¹,

Pathak²

2008

Science and Technology of Advanced Materials

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“…A variety of bases, including Ph,CNa (36), Na (14a), NaH (14a), LiOH (14a), K O H (15), n-Bu4NOH (1 l ) , EtLi (14a), n-BuLi (37), Ph,P=CH2 ( l o ) , NaNH, (14a), and liquid ammonia (17,20) have been used for the deprotonation of S7NH. The available evidence indicates that the yellow S7N-ion is thermally stable below -50°C in T H F (1 l~, 15), but it decomposes to give the blue SSNSS-ion above this temperature (1 1 at -364 ppm.…”

Section: Nmr Characterization Of the Sn-ionmentioning

confidence: 99%

“…been suggested on the basis of UV-visible (19,20) and Investigations of binary sulphur-nitrogen (S-N) anions have contributed significantly to the development of S-N chemistry (1). The well-characterized examples include cyclic anions, S,N,-and S4N5-(2, 3), acyclic catenated anions, SSNSS-and SSNS- (4,5), and the dianion NSN" (6).…”

Section: Introductionmentioning

confidence: 99%

“…The formation of the S7N-ion in sulphur-ammonia solutions (SAS) has also been the controversial subject of several recent investigation~ (16)(17)(18). Finally, the possible production of the S2N-ion from the electrochemical reduction (19) of SNSS-or the reaction of SNSS-with amide ion (20) has '~u t h o r to whom correspondence may be addressed.…”

Section: Introductionmentioning

confidence: 99%

“…Raman s~c t r o s c o p i c evidence (20). Several recent publications have demonstrated the value of ',N NMR spectroscopy for monitoring the behavior of small S-N molecules or ions in solution (2 1-25).…”

Section: Introductionmentioning

confidence: 99%

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Sulphur–nitrogen anions: ¹⁴N and ¹⁵N NMR investigations of the deprotonation of cyclic sulphur imides and sulphur–ammonia solutions

Chivers¹,

Schmidt²

1992

Can. J. Chem.

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The following systems have been investigated by 1 4~ and ( o r ) 1 5~ NMR spectroscopy: (a) the deprotonation of S7NH by n-BuLi, (b) solutions of S,, S7NH, 1,3-and 1 ,4-S6(NH),, and K2SNZ in liquid ammonia, (c) the reaction of sodium azide with sulphur in hexamethylphosphoramide (HMPA), (4 the reactions of S7NH and S4(NH), with potassium amide in liquid ammonia in various molar ratios, and (e) the reaction of (NSCI), with potassium amide (1 :6 molar ratio) in liquid ammonia. These investigations have provided an NMR characterization of the thermally unstable S7N-( 6 "~ ca.-324 ppm) and S2N2H-ions ( 6 1 4~ + 7 and -149 ppm, 'J('~N-'H) 36 Hz, 'J("N-H) 55 Hz, -J("N-'~N) 2.2 Hz) in liquid ammonia, demonstrated the existence of S7N-, in addition to SSNSS-, as the major nitrogen-containing ingredient of sulphur-ammonia solutions (SAS), and confirmed the formation of the SSNSS-, but not S7N-, from the reaction of sodium azide and sulphur in HMPA. Consistent with previous chemical investigations, the NMR data show that the S7N-and S,N,H-ions are thermally unstable with respect to the formation of SSNSS-and S,N,-, respectively, in solution. Solutions of S4(NH),/4KNHI or (NSC1),/6KNH2 show the same two "N or "N NMR resonances at ca. +97 and -108 ppm as a solution of NSN'-in liquid ammonia.

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From Ammonia

Chivers¹

1991

Inorganic Reactions and Methods

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Chemical species in sulfur-ammonia solutions: influence of amide addition

Cited by 25 publications

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Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Sulphur–nitrogen anions: ¹⁴N and ¹⁵N NMR investigations of the deprotonation of cyclic sulphur imides and sulphur–ammonia solutions

From Ammonia

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Chemical species in sulfur-ammonia solutions: influence of amide addition

Cited by 25 publications

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Microwave-assisted synthesis of WS2nanowires through tetrathiotungstate precursors

Microwave-assisted synthesis of WS2nanowires through tetrathiotungstate precursors

Sulphur–nitrogen anions: 14N and 15N NMR investigations of the deprotonation of cyclic sulphur imides and sulphur–ammonia solutions

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Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Microwave-assisted synthesis of WS₂nanowires through tetrathiotungstate precursors

Sulphur–nitrogen anions: ¹⁴N and ¹⁵N NMR investigations of the deprotonation of cyclic sulphur imides and sulphur–ammonia solutions