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However, optimizing the solvothermal process by altering the solvent mixture has not attracted much attention. According to previous reports [ 39 , 40 ], syntheses in mixed solvents favor the formation of nanostructures with more uniform sizes and uncommon architectures compared with syntheses in single solvents.
Most reports have focused on the synthesis of Bi 2 S 3 in water [ 19 , 22 , 23 , 25 , 27 , 34 , 38 , 41 ].
The usage of other solvents, including ethanol [ 21 ], ethylene glycol [ 20 ] or glycerol [ 36 ], has been rarely reported. Butyldiglycol, also known as diethylene glycol butyl ether, is an inexpensive solvent that is easily miscible with water and used in many commercial products.
Despite its interesting surfactant-like properties, butyldiglycol has not yet been used in the synthesis of metal sulfides.
This is the first time such a high capacitance value has been demonstrated for a Bi 2 S 3 electrode. The mass ratio of bismuth salt to thioacetamide was equal to 6.
Briefly, the experimental procedure was as follows. To determine the surface elemental composition and valence states of Bi and S in the products, X-ray photoelectron spectroscopy XPS analyses were performed using a PHI VersaProbe instrument.
The specific surface area and pore size distribution of the Bi 2 S 3 samples were evaluated applying the Brunauer—Emmett—Teller BET and quenched solid-state functional theory QSDFT methods, respectively.
The Dubinin—Radushkevich equation was used to assess the micropore volume V mic. The mesopore volume V mes was evaluated as the difference between V T and V mic.
The crystalline structure of the as-synthesized Bi 2 S 3 samples was determined by XRD. The peak locations at 2 theta of The sharp peaks prove that high crystallinity Bi 2 S 3 is successfully synthesized using the applied process.
Furthermore, secondary crystalline phases, such as crystalline bismuth, sulfur or bismuth oxide, are not present, indicating the high purity of the resulting products.
As follows from the XRD patterns in Fig. The crystallite size of Bi 2 S 3 was evaluated for the peak with the highest intensity, recorded at 2 theta of The detailed surface composition of the obtained products was examined by XPS.
The XPS survey spectra Fig. The chemical state of Bi 2 S 3 was further investigated by high-resolution Bi 4 f and S 2 p XPS spectra Fig.
The Bi 4 f spectrum of Bi 2 S 3 -W Fig. The Bi 4 f spectra of the other samples show peaks at Moreover, the nearly symmetric shape of these signals without distinct distortions at their shoulders excludes the presence of metallic Bi and Bi 2 O 3 , which would appear at The spin—orbit doublet of S 2 p overlaps with the Bi 4 f region.
To distinguish between the regions, the magnified core-level S 2 p spectrum is shown below the Bi 4 f region for each Bi 2 S 3 sample.
The S 2 p region consists of two asymmetric peaks. However, the smaller signal at approximately The S 2 p peaks are at and The Bi 2 S 3 samples were further investigated by FESEM and HRTEM to determine the influence of the solvent on their morphology and microstructure.
The solvent is a critical parameter in a solvothermal synthesis that affects the morphology and size of the growing Bi 2 S 3 particles. Help Print this page.
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