Matrix-assisted laser desorption/ionization (MALDI)
and Fourier-transform ion cyclotron
mass spectrometry (FT-ICR-MS) are combined for the characterization of
polyoxyalkyleneamines. 1H
and 13C NMR data are used to confirm and quantify
structural assignments. Characterization of the
molecular weight distribution, chemical composition distribution, and
end group distribution of amine-terminated (co-)polymers of ethylene oxide and propylene oxide is
rather complex because the convolution
of these three entities yields an ensemble of structurally related
molecules which is hard to characterize
by conventional analytical techniques. In this study MALDI
FT-ICR-MS is used to resolve intact, Na+
cationized, oligomer ions in the mass range from m/z 500 to
3500. This revealed the presence of various
compositional distributions in the polyoxyalkyleneamines. The
individual compound masses in the
molecular weight distributions were measured with a mass accuracy of
<20 millimass units, allowing
end group and repeat unit determination with an accuracy of better than
50 millimass units. NMR is
used to measure the average end group distribution to provide insight
in conformational differences. In
this respect, FT-ICR-MS data and NMR data are complementary. The
combined results yield detailed
information about chemical composition distributions of
polyoxyalkyleneamines that hitherto it was not
possible to obtain with either technique separately.
A novel low temperature process for titanium nitride (TiN) deposition by means of an electron cyclotron resonance (ECR) plasma CVD process was applied to poly(tetrafluoroethylene) (PTFE). The organometallic compound tetrakis(dimethylamido)titanium (TDMAT) introduced into the downstream region of a nitrogen ECR plasma was used as a precursor for TiN deposition at 100°C.The thin TiN films (thickness 15-30 nm) act as interlayers to activate the electroless deposition of copper followed by an electroplating process. Prior to the deposition of the interlayer, the samples were treated on a biased susceptor with argon ions to enhance the adhesion of the TiN interlayer. This metallization procedure avoids the use of toxic and pollutive etching agents and yields adherent copper layers on PTFE.The maximum adhesion of the metal film on PTFE was established to be 13 N/mm2. As shown by atomic force microscopy (AFM), TiN grains were formed on the fluoropolymer surface. Film composition was investigated by secondary ionization mass spectrometry (SIMS).
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