Double shadow masking sample preparation method for in‐situ TEM characterization

Abstract

A novel double mechanical masking-based sample preparation method is introduced for in-situ transmission electron microscopy (TEM) characterizations. In the current study amorphous vanadium pentoxide thin film deposition is carried out by using the developed double mask on a transparent window of TEM chip on precisely selected spots by a reactive sputtering technique. The prepared sample is less damaged since it is not subjected to ion beam exposure. And the probability of achieving a viable TEM sample is also enhanced compared to classical preparation methods. In-situ temperature-based electron diffraction pattern sequences are recorded for amorphous vanadium pentoxide in the temperature region of 25 to 500˚C. This allowed observing the crystallization temperature at ∼416˚C. The pre-and post-heat-treated microstructure and electron diffraction pattern of the vanadium pentoxide thin film showed the formation of a mixed crystalline and amorphous film. Thus, a most reliable, reusable and cost effective TEM sample preparation method was demonstrated. K E Y W O R D S amorphous crystalline behavior, double masking techniques, electron diffractions, in-situ transmission electron microscopy, vanadium pentoxide (V 2 O 5) This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.

Interface‐Driven Thermoelectric Switching Performance of VO+‐Diffused Soda‐Lime Glass

“…Furthermore, the thermal behavior of the thin-film/ glass system is highly reversible and stable. Recent in situ TEM work [32] illustrates that no bulk transitions, such as an oxidation state change or the crystallization of the amorphous vanadium pentoxide thin film, occur below 400 C. Permanent vanadium oxidation state intensity changes were not observed in the depth profiles obtained by ToF-SIMS. For the first time, the production of interface-confined NaVO þ via a solid-state thermal reaction of vanadium pentoxide with sodium ions supplied by the soda-lime glass substrate is documented.…”

Demystifying the Semiconductor‐to‐Metal Transition in Amorphous Vanadium Pentoxide: The Role of Substrate/Thin Film Interfaces

“…The observed process was reversible and is reported to involve a significant modification of the coordination of V 4+ . As mentioned earlier, the decomposition and the associated formation of a reduced oxidation state were reported to occur at temperatures above 400 °C in a high vacuum environment for crystalline V 2 O 5 , [ 43,44,53 ] therefore the current investigation has been limited to temperatures below 400 °C.…”

“…[ 27 ] The detailed sample preparation method and the demonstration of its usage are presented elsewhere. [ 53 ]…”

“…[27] The detailed sample preparation method and the demonstration of its usage are presented elsewhere. [53] EELS low-loss and high-loss spectra were obtained in the energy window of 0-200 eV and 500-700 eV, respectively. The temperature was controlled by the Protochip fusion software via a Keithley sourcemeter.…”

Comparative microstructural analysis of V2O5 nanoparticles via x-ray diffraction (XRD) technique

“…Vanadium pentoxide also plays a crucial role in opticalelectrical and electrochromic applications when doped with certain elements [13]. Its optical properties make it suitable for use in solar cells, where it can contribute to enhancing energy conversion efficiency [14]. Additionally, vanadium pentoxide has been investigated for its potential in cancer diagnosis and treatment, serving as tumor therapeutic and diagnostic agents [15].…”