期刊
CHEMICAL VAPOR DEPOSITION
卷 17, 期 4-6, 页码 162-169出版社
WILEY-BLACKWELL
DOI: 10.1002/cvde.201106909
关键词
Alumina; Molybdenum trioxide; Mo(CO)(6); Rotating hot-wall reactor; Shell-core composites; X-ray photoelectron spectroscopy
资金
- German Research Foundation (DFG) [MU 1327/5-1]
MoO3/gamma-Al2O3 composites are synthesized by CVD under atmospheric pressure using Mo(CO)(6) as the precursor and porous gamma-Al2O3 particles in a horizontal, rotating, hot-wall reactor, which is also used for calcination in air. The composites are characterized by N-2 physisorption, atomic absorption spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), and laser Raman spectroscopy (LRS). The synthesized samples exhibit excellent porosity, even at high Mo loadings. A much higher Mo yield is achieved when applying sublimation-adsorption in static air instead of using flowing N-2. A high degree of Mo dispersion on alumina is confirmed by XRD, LRS, and TEM; with a Mo surface density as high as 5.2 atoms nm(-2), the sample is X-ray amorphous, there are no polymeric molybdate species detectable by LRS, and the island size of the molybdate species is about 1 nm according to TEM. The XPS analysis shows that exclusively Mo-VI species are present on all synthesized samples. Thus, the applied rotating, hot-wall reactor achieves efficient mixing and homogeneous deposition.
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