Abstract
The ability of electrons and atomic hydrogen (AH) to remove residual chlorine from PtCl2 deposits created from cis-Pt(CO)2Cl2 by focused electron beam induced deposition (FEBID) is evaluated. Auger electron spectroscopy (AES) and energy-dispersive X-ray spectroscopy (EDS) measurements as well as thermodynamics calculations support the idea that electrons can remove chlorine from PtCl2 structures via an electron-stimulated desorption (ESD) process. It was found that the effectiveness of electrons to purify deposits greater than a few nanometers in height is compromised by the limited escape depth of the chloride ions generated in the purification step. In contrast, chlorine atoms can be efficiently and completely removed from PtCl2 deposits using AH, regardless of the thickness of the deposit. Although AH was found to be extremely effective at chemically purifying PtCl2 deposits, its viability as a FEBID purification strategy is compromised by the mobility of transient Pt–H species formed during the purification process. Scanning electron microscopy data show that this results in the formation of porous structures and can even cause the deposit to lose structural integrity. However, this phenomenon suggests that the use of AH may be a useful strategy to create high surface area Pt catalysts and may reverse the effects of sintering. In marked contrast to the effect observed with AH, densification of the structure was observed during the postdeposition purification of PtCx deposits created from MeCpPtMe3 using atomic oxygen (AO), although the limited penetration depth of AO restricts its effectiveness as a purification strategy to relatively small nanostructures.
Highlights
Focused electron beam induced deposition (FEBID) has demonstrated great potential in the field of nanostructure fabrication [1,2,3,4]
atomic hydrogen (AH) was found to be extremely effective at chemically purifying PtCl2 deposits, its viability as a focused electron beam induced deposition (FEBID) purification strategy is compromised by the mobility of transient Pt–H species formed during the purification process
In marked contrast to the effect observed with AH, densification of the structure was observed during the postdeposition purification of PtCx deposits created from MeCpPtMe3 using atomic oxygen (AO), the limited penetration depth of AO restricts its effectiveness as a purification strategy to relatively small nanostructures
Summary
Focused electron beam induced deposition (FEBID) has demonstrated great potential in the field of nanostructure fabrication [1,2,3,4]. The precursor decomposes under electron beam irradiation, with non-volatile product species being incorporated into the growing deposit. Some purification approaches that remove chemical impurities and decrease metal content negatively impact the shape integrity of the deposits by producing voids, cracks or other unwanted side effects [5,9,10,14,15]. An ideal purification strategy in FEBID is one that removes all of the organic impurities to leave behind a compact, high-fidelity metal nanostructure, whose shape is unchanged as compared to the as-deposited structure. Approaches which have been attracting increased interest are the so-called “low temperature” purification strategies, where carbon is removed at temperatures low enough to avoid changing the structure and morphology of the deposit
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