Coatings are of increasing importance for many industrial products for reasons of decoration as well as stability.
There is a technological challenge caused by various substrates used (e.g. metals, glass, polymers), because different classes of material are applied as coatings, and because many products are reshaped after the coating step.
Crater formation and adhesion problems are therefore among the most common analysis requests.
Car Paint Cross-section
The example shows the chemical composition of a paint cross-section.
The images show the distribution of the different SO3 and Cl representing the different layers as well as the allocation of the imbeded hindered amine light stabilizers (HALS) and UV adsorbers (UVA).
HALS + UVA
Time-of-Flight secondary ion mass spectrometry (TOF-SIMS) is a very sensitive surface analytical technique, well established for many industrial and research applications. TOF-SIMS is an acronym for the combination of the analytical technique SIMS (Secondary Ion Mass Spectrometry) with Time-of-Flight mass analysis (TOF). The technique provides detailed elemental and molecular information about the surface, thin layers, interfaces of the sample, and gives a full three-dimensional analysis. The use is widespread, including semiconductors, polymers, paint, coatings, glass, paper, metals, ceramics, biomaterials, pharmaceuticals and organic tissue.
For a TOF-SIMS analysis, a solid surface is bombarded by primary ions of some keV energy. The primary ion energy is transferred to target atoms via atomic collisions and a so-called collision cascade is generated.
Part of the energy is transported back to the surface allowing surface atoms and molecular compounds to overcome the surface binding energy. The interaction of the collision cascade with surface molecules is soft enough to allow even large and non-volatile molecules with masses up to 10,000 u to escape without or with little fragmentation. SIMS is a very surface sensitive technique because the emitted particles originate from the uppermost one or two monolayers.
Most of the emitted particles are neutral in charge, but a small proportion is also positively or negatively charged.
The subsequent time-of-flight mass analysis of the emitted ions provides detailed information on the elemental and molecular composition of the surface.
TOF mass spectrometry is based on the fact that ions with the same energy but different masses travel with different velocities.
An electrostatic field accelerates the generated ions to a common energy.
The accelerated ions then travel over a drift path to the detector. The lighter ions fly with a higher velocity and arrive at the detector before the heavier ions. Measuring the flight time for each ion allows the determination of its mass. This cycle is repeated with a repetition rate of up to 50 kHz.
Modern TOF analysers compensate the small differences in initial energy and angle of the ions in order to achieve high mass resolution. The combination of a linear drift path and an ion mirror (reflectron) allow for mass resolutions (M/dM) of above 18,000.
Major advantages of this approach over quadrupole and magnetic sector type analysers are the extremely high transmission, the parallel detection of all masses and the unlimited mass range.
The pulsed primary ion beam can be focussed to a small spot (microprobe mode) and rastered to determine the lateral distribution of elements and molecules. In this mode of operation lateral resolution of down to 50 nm can be achieved.
During the drift time of the secondary ions, the extraction field is switched off and low energy electrons can be used to compensate for any surface charging caused by primary or secondary particles (charge compensation). Thus all types of bulk insulators can be analysed without any problems.
The time during which the extraction field is switched off can also be used to apply low energy ion beams for sample erosion.
In this case the low energy beam forms a sputter crater, the centre of this crater is analysed by the pulsed primary ion beam (dual beam depth profiling).
The aim of a static SIMS investigation is the analysis of the original, non-modified surface composition. As SIMS in principle is a destructive technique this means that the contribution of those secondary ions to the spectrum originating from already bombarded surface areas to the spectrum must be negligible. This quasi non-destructive surface analysis can be achieved by the application of very low primary ion dose densities. Surface Spectroscopy provides detailed elemental and molecular information from the outer monolayers.
By rastering a fine-focussed ion beam over the surface, like an electron beam in an electron microprobe, mass resolved secondary ion images (chemical maps) can be obtained simultaneously.
For Depth Profiling two ion beams operate in the Dual Beam Mode. While the first beam is sputtering a crater, the second beam is progressively analysing the crater bottom.
The visualisation of 3D sample structures is possible by combining spectral, imaging and depth information. 3D Analysis is ideal for the investigation of complex and unknown structures or defects. In particular the composition, shape and position of features and defects can be visualised.
As well as comprehensive on-line analysis, the parallel mass detection of the TOF.SIMS 5 and the TOF.SIMS 300 provides the means to carry out Retrospective Analysis.
Regardless of the knowledge about the sample before the measurement, the data can be explored afterwards to look for unexpected results, such as unknown structures, contaminants at interfaces and so on.
The software can reconstruct spectra from any coordinate or group of coordinates, images from any section, vertical or horizontal, depth profiles from any selected area and various 3D views as required.
High sensitivity in the ppm/ppb range
High mass resolution and accuracy even on insulating samples
High mass range
High lateral resolution (<60 nm)
Fast image acquisition (up to 50 kHz pixel frequency)
Field of view from µm2 to cm2
Depth resolution better than 1 nm
High mass resolution
Sputter speed of up to 10 µm/h
Ideally suited for insulators
Manufactured structures: TFT displays...
Defect Analysis: buried particles...
Material Science: grain boundaries, diffusion...
Parallel mass detection
High depth resolution
High image resolution
The x, y, z coordinates and mass of every secondary ion reaching the detector are stored.