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

Abstract

AbstractA 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.