研究目的
To acquire a better understanding of the basic and the modulated structures of NbS3-II through a combination of synchrotron x-ray powder diffraction, high-resolution scanning transmission electron and scanning tunneling microscopy studies, ab initio calculations, and simulation of electron diffraction patterns.
研究成果
The study confirmed the basic structure of NbS3-II and proposed models for the CDW modulation patterns. The basic structure belongs to the space group P 21/m, and the CDWs are ordered according to one of two possible modulation pattern space groups, Cm or C2/m. The entire modulated structure can be described as a long-period commensurate superstructure with both CDWs included.
研究不足
The study was limited by the small size and hairlike morphology of NbS3-II crystals, their tendency to bend, and a slight nonstoichiometry of about 3% S deficiency. These factors prevented the basic and CDW-modulated structures from being accurately determined by means of single-crystal x-ray analysis alone.
1:Experimental Design and Method Selection
The study employed synchrotron x-ray diffraction, ab initio calculations, simulation of electron diffraction patterns, atomic-resolution transmission electron microscopy, and low-temperature scanning tunneling microscopy to investigate the basic and CDW structures of NbS3-II.
2:Sample Selection and Data Sources
NbS3-II whiskers were grown in a three-zone furnace with separate temperature control for each zone. Samples were prepared by carefully cutting the whiskers and packing them into borosilicate capillaries for XRD experiments.
3:List of Experimental Equipment and Materials
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4:Experimental Procedures and Operational Workflow
The NbS3-II whiskers were grown and prepared for analysis. HR STEM images were acquired with an aberration-corrected probe. STM was conducted on freshly cleaved samples in ultrahigh vacuum. XRD experiments were performed with the samples packed into capillaries and kept spinning during data collection.
5:Data Analysis Methods
The diffraction patterns were analyzed with the Le Bail and Rietveld methods using the Bruker DIFFRAC.TOPAS program. DFT calculations were performed using the QUANTUM ESPRESSO code with GBRV ultrasoft pseudopotentials and the PBE functional.
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