A thin Fe2TiO5 layer was produced on hematite either by evaporating a TiCl4 solution on FeOOH or by a simple HF-assisted Ti treatment of FeOOH, both followed by annealing. The prepared Fe2TiO5-hematite heterostructure showed a significant enhancement in photocurrent density compared to that of the pristine hematite. For example, the sample after HF-assisted Ti treatment exhibited a significantly enhanced photocurrent of 2.0 mA/cm(2) at 1.23 V vs RHE. Moreover, the performance of the Fe2TiO5-hematite heterostructure can be further improved by coupling with Co-Pi catalysts, achieving a higher photocurrent of 2.6 mA/cm(2) at 1.23 V vs RHE. Synchrotron-based soft X-ray absorption spectroscopy analyses clearly revealed the existence of an Fe2TiO5 structure on hematite forming a heterojunction, which reduced the photogenerated hole accumulation and then improved the performance.

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The identification of effective components on the atomic scale in carbon nanomaterials which improve the performance in various applications remains outstanding challenges. Here the catalyst residues in individual carbon nanotube (CNT) and carbon nanofiber (CNF) were clearly imaged with a concurrent characterization of their electronic structure by nanoscale scanning transmission X-ray microscopy. Except for prominent catalyst nanoparticle at the tip, tiny catalyst clusters along the tube (fiber) were detected, indicating a migration of the catalysts with the growth of CNTs (CNFs). The observation provides the direct evidence on the atomic metal in CNT for oxygen reduction reported in the literature. Interaction between catalysts (Fe, Ni) and CNTs (CNFs) at the tip was also identified by comparing the X-ray absorption spectra. A deep understanding of catalyst residues such as Fe or Ni in carbon nanomaterials is very vital to growth mechanism development and practical applications.

We have stabilized the iron oxide nanoparticles (NPs) of various sizes on layered carbon materials (Fe-oxide/C) that show excellent catalytic performance. From the characterization of X-ray absorption spectroscopy (XAS), X-ray emission spectroscopy (XES), scanning transmission X-ray microscopy (STXM) and X-ray magnetic circular dichroism spectroscopy (XMCD), a strong interfacial interaction in the Fe-oxide/C hybrids has been observed between the small iron oxide NPs and layered carbon in contrast to the weak interaction in the large iron oxide NPs. The interfacial interaction between the NPs and layered carbon is found to link with the improved catalytic performance. In addition, the Fe L-edge XMCD spectra show that the large iron oxide NPs are mainly γ-Fe2O3 with a strong ferromagnetic property, whereas the small iron oxide NPs with strong interfacial interaction are mainly α-Fe2O3 or amorphous Fe2O3 with a nonmagnetic property. The results strongly suggest that the interfacial interaction plays a key role for the catalytic performance, and the experimental findings may provide guidance toward rational design of high-performance catalysts.

The electronic structure of individual multi-walled carbon nanotubes (MWCNTs) has been probed using scanning transmission X-ray microscopy (STXM). Although transmission electron microscope (TEM) images show that the exterior of the MWCNTs are clean and straight; the inside structure of some of the MWCNTs is much less well ordered, as revealed by STXM. The amorphization of the interior tubes can be introduced in the growth or modification processes. Moreover, TEM measurement with high dose may also lead to the inside damage. Our results reveal that the structure of individual MWCNTs can be complex and suggest that electronic structure measurements are an important tool for characterizing carbon nanomaterials.