In situ temperature-time effect on MetA-S-SIMS

Metal-assisted (MetA) static secondary ion mass spectrometry (S-SIMS) is one of several ion yield enhancing methods developed for S-SIMS in the last decades. MetA-S-SIMS uses a very thin coating of gold or silver on the sample. Earlier experiments revealed dependence of the ion yield enhancement on the applied metal, the nature of the studied sample, the time after metallization, and the heating temperature (ex situ, i.e., under atmospheric pressure). This paper reports on the effects of time and temperature when samples are heated to temperatures between 30 and 80 °C inside the S-SIMS vacuum chamber (in situ). Thick layers of poly(vinylbutyral-co-vinylalcohol-co-vinylacetate) (PVB) containing dihydroxybenzophenone (DHBPh) were coated with a nm-thin-layer of gold. The S-SIMS analysis was performed over a period of several hours while samples were kept at a constant elevated temperature. Compared to ex situ heating in an oven, heating in the analysis chamber provided more rapid signal enhancement, but the magnitude of the enhancement was less (by a factor of two). Furthermore, additional experiments on ex situ heated samples revealed that storage of samples with enhanced ion yields at −8 °C is not sufficient to “stabilize” the enhancement. A steep decrease of the ion yields was observed as a function of time after 2.5 h.