Direct Measurements of the Radiolytic Transformation of Thin Films of Titanium Dioxide using EELS

Rez, Peter; Weiss, J. K.; Medlin, Douglas L.; Howitt, D. G.

doi:10.1051/mmm:1995133

Cited by 13 publications

(13 citation statements)

References 16 publications

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“…The absence of splitting has already been reported as well for amorphous, i. e. disordered, Ti02 [13] as for substoichiometric TiOx. However in the latter case a shift of the Ti L2,3 edge should be observed [14]. In the present study, no detectable shift has been found in the neighbourhood of the interface, confirming the hypothesis of the existence of a Ti02-Si02 solid solution.…”

Section: Expérimental Resultssupporting

confidence: 77%

“…Simultaneously, one notices the disappearance of the splitting on Ti L2,3 and 0 K edges, as well as the decay of the extended fine structure of Ti L2,3 edge. As no shift on the Ti L3 edge position is observed, contrary to the case investigated in reference [14] where this shift was explained by a reduction of Ti02 down to TiO, it is likely that the damage observed in the present work only involves an amorphization process. As a matter of fact, Rez et In a further step, it would be necessary to investigate, within the relevant range of electron doses, how the different materials behave as a function of local thickness.…”

Section: Expérimental Resultscontrasting

confidence: 52%

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Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface

Brun

Colliex

Rivory

et al. 1996

Microsc. Microanal. Microstruct.

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Abstract. 2014 SiO2/TiO2 multilayers stacks used in optical coatings have been studied by Electron Energy Loss Spectroscopy (EELS). The line-spectrum mode has been used: the incident electron probe of the STEM is scanned under digital control on the specimen surface in the direction perpendicular to the layers, while the whole spectrum is acquired. The selected energy range contains Ti L23 and O K edges, in order to study the evolution of the fine structures visible on these edges. Every experimental spectrum is then fitted with a linear combination of the two reference spectra (TiO2 and SiO2) extracted from the same sequence. It is possible to identify in the neighbourhood of the interface some EELS fine structures which cannot be fitted to a combination of reference spectra, but are representative of hybrid environments, such as Si-O-Ti in the present study. A quantitative analysis of the changes in different fine structures on the titanium and oxygen edges enables to clearly discriminate different levels of interdiffusion at the boundary.

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Section: Expérimental Resultssupporting

confidence: 77%

Section: Expérimental Resultscontrasting

confidence: 52%

Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface

Brun

Colliex

Rivory

et al. 1996

Microsc. Microanal. Microstruct.

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“…This is mainly attributed to the presence of an amorphous layer on the top and bottom surfaces of the specimen. The observed shape is similar to those observed for amorphous titanium oxide (Berger et al ., 1987; Rez et al ., 1995).…”

Section: Resultsmentioning

confidence: 99%

Advances in EELS spectroscopy by using new detector and new specimen preparation technologies

Scheu¹,

Gao²,

Benthem³

et al. 2003

Journal of Microscopy

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SummaryFirst results obtained with a Gatan UHV Enfina system, which was attached to a VG HB 501 UX dedicated STEM, are reported. The Enfina system is based on a CCD detector and offers, compared to the previously used photodiode array, a narrower point-spread function, higher sensitivity, and faster read-out capabilities. These improvements are demonstrated with electron energy-loss measurements on various oxides, such as Al 2 O 3 , TiO 2 and SrTiO 3 . It is shown that a better energy resolution is achieved and that acquisition of high-energy absorption edges with a reasonable signal-to-noise ratio becomes possible. Furthermore, we report on the influence of the TEM specimen quality on the energy-loss spectra. Thin amorphous layers at the specimen surfaces, which are induced by ion-milling processes, can modify specific electron energy-loss near-edge structure features. We found that for the investigated ceramics the use of low-energy ion-milling systems is highly recommended, since the loss of energy-loss near-edge structure details by the presence of the amorphous layers is considerably reduced. This is especially true for very thin specimens.

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“…We would like to revisit this topic with the specific focus of High resolution EELS of this transformation and general cautionary commentary on STEM work in nanostructures. If the beam is rapidly scanned over a region such as a line or square (as indicated in Fig 1), the observed spectra (Fig 2) is typical of anatase TiO 2 with the B peak split into B 1 and B 2 and B 1 showing up stronger than B 2 [2]. In Fig 2, this is only seen as the peak at the B 1 position and an asymmetry in the B peak.…”

mentioning

confidence: 87%

“…

In 1995 Peter Rez et al discussed the Radiolytic transformation of TiO 2 to TiO under high flux electron irradiation (~10 8 A/m 2 ) as observed from the fine structure changes in Electron Energy Loss Spectra (EELS) [1]. We would like to revisit this topic with the specific focus of High resolution EELS of this transformation and general cautionary commentary on STEM work in nanostructures.

…”

mentioning

confidence: 99%

Radiolytic Transformation of TiO2 Revisited with High Resolution EELS

Neff

Vanfleet

2005

MAM

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In 1995 Peter Rez et al. discussed the Radiolytic transformation of TiO 2 to TiO under high flux electron irradiation (~10 8 A/m 2 ) as observed from the fine structure changes in Electron Energy Loss Spectra (EELS) [1]. We would like to revisit this topic with the specific focus of High resolution EELS of this transformation and general cautionary commentary on STEM work in nanostructures. If the beam is rapidly scanned over a region such as a line or square (as indicated in Fig 1), the observed spectra (Fig 2) is typical of anatase TiO 2 with the B peak split into B 1 and B 2 and B 1 showing up stronger than B 2 [2]. In Fig 2, this is only seen as the peak at the B 1 position and an asymmetry in the B peak. However, when the beam is stopped at the center of the circle shown in Fig 1, the spectra shifts to lower energy onset and loses the clear A -B set of peaks. This new fine structure appears to be two peaks separated by less than 1 eV. Peak labeling follows the A, B pattern of reference 2.Both spectra shown in Fig 2 were taken at 6 seconds of integration time. However, the electrons involved in the "area" spectra are spread over a region greater than 100 times as large as the spot spectra with an expected corresponding greater than 100 fold decrease in the damage rate. However, in the case of the stopped beam, the damage rate is significantly faster than that seen by Rez [1]. This difference in damage rate could be attributed to difference in electron dose. However, similar data from single crystal anatase particles of similar overall size (~70-100 nm) show no damage on the six second time scale. This indicates a significant enhancement of the damage rate due to the small size and resulting large surface of the fundamental constituent particles.This underscores and illustrates that we must be careful to both minimize and understand the role of beam damage when using the extremely high electron density probes seen in STEM work [3].

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Direct Measurements of the Radiolytic Transformation of Thin Films of Titanium Dioxide using EELS

Cited by 13 publications

References 16 publications

Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface

Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface

Advances in EELS spectroscopy by using new detector and new specimen preparation technologies

Radiolytic Transformation of TiO2 Revisited with High Resolution EELS

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Direct Measurements of the Radiolytic Transformation of Thin Films of Titanium Dioxide using EELS

Cited by 13 publications

References 16 publications

Spatially Resolved EELS Fine Structures at a SiO2/TiO2 Interface

Spatially Resolved EELS Fine Structures at a SiO2/TiO2 Interface

Advances in EELS spectroscopy by using new detector and new specimen preparation technologies

Radiolytic Transformation of TiO2 Revisited with High Resolution EELS

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Product

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Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface

Spatially Resolved EELS Fine Structures at a SiO₂/TiO₂ Interface