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Time-of-flight static secondary ion mass spectrometry as an analytical tool to obtain molecular information on and in organic materials

Posted on:2007-01-10Degree:Ph.DType:Dissertation
University:Universiteit Antwerpen (Belgium)Candidate:Adriaensen, LesleyFull Text:PDF
GTID:1441390005465641Subject:Chemistry
Abstract/Summary:
The fast progress in material and human science puts high demands on analytical techniques. To fully understand the working principles of materials, detailed structural information on a small scale (nm), is often needed. In this work a methodology is developed which uses time-of-flight static secondary ion mass spectrometry (TOF-S-SIMS) to obtain molecular information on and in organic materials with a lateral resolution below 1 mum. Two important issues are addressed, the optimization of sample preparation methods and the enhancement of secondary ion yields.; In first instance a series of organic fluorinated carbocyanine dyes, containing cationic, anionic and zwitterionic dyes with similar structures, and the pharmaceutical Risperidone were measured with different primary ion guns (Ga+, SF5+, Aun +), on different substrates (Si, Ag, PET,...) and embedded in several polymer matrices, in order to get more insight on their behaviour under primary ion bombardment. By using the desorption-ionisation model (DI) it was possible to produce tentative fragmentation pathways and assign the most important ion signals in the recorded spectra with a mass accuracy of at least 50 ppm.; TOF-S-SIMS is a surface sensitive technique, so to obtain data of the deeper layers, a suitable sample preparation technique is needed. In this context several methods were tested, laserablation, cross section polisher (CSP), glow discharge, microtomy and focused ion beam milling (FIB).; Organic molecules generally give low secondary ion yields when measured with TOF-S-SIMS, so a method is needed that can induce an enhancement of the organic ion yields. Two methods were studied in this regard, namely, matrix-enhanced SIMS (ME-SIMS) and metal-assisted SIMS (MetA-SIMS). In ME-SIMS the analyte is mixed with a suitable MALDI matrix which resulted in enhancement factors between 4 and 45. For the MetA-SIMS method a thin layer (3-5 nm) of noble metals (Au, Ag) is deposited onto the sample surface prior to the measurement. This gives rise to enhancement factors of 100 and more.; The knowledge, obtained during sample preparation experiments and MetA-SIMS experiments was combined to do some measurements in cross sections of organic materials consisting of one or more layers.
Keywords/Search Tags:Ion, Organic, Materials, Obtain, Mass
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