Screening of properties of formulations and coatings is an important but often time-consuming step of material research programs. To be able to screen the high number of samples FLAMAC has worked together with different suppliers of screening equipment to automate and where possible accelerate their instrumentation. This allows external companies to outsource some of their screening experiments in an economically viable way at Flamac.
Automated X-ray structure analysis
Instrument: Bruker Discovery D8 with Vantec 2D detector / Automated up to 96 samples
X-ray diffraction techniques are well known and commonly used to determine the crystallographic structure, the chemical composition and physical properties of materials and thin films.
XRD (X-ray diffraction) allows for rapid, non-destructive analysis without the need for extensive sample preparation. Due to the interaction between the X-ray beam and the tested material a diffraction pattern is recorded by the CCD camera. This pattern reveals information about the crystallinity of the structure and can provide identification information after comparing with known patterns from databases.
This instrument is specially adapted for accelerated measurements. The time to perform an experiment is significantly decreased by the use of the unique Vantec 2000 2D detector.
Additionally this instrument can be equipped with a 96 position tray which allows unattended automated experiments overnight.
XRR (x-ray reflectometry) is a surface-sensitive analytical technique used to characterize surfaces, thin films and multilayers. The intensity of the x-ray beam that is reflected by a surface reveals information about the density, thickness and smoothness of the surface.
Applications: Inorganic coatings / Pharmaceutical compounds / Thin films / Catalysts / Ceramics / Powders / Alloys
Instrument: Sentech SE 850 / Automated up to 24 samples
Ellipsometry is a versatile non-destructive and powerful optical technique for the investigation of the dielectric properties of thin films. It is based on the change of polarization of light, which is reflected off the surface of a sample. It is mostly used to characterize film thickness and optical properties of single or complex multilayer’s ranging from a few angstroms (0,1 nm) to several micrometers with an excellent accuracy.
The instrument at FLAMAC has been adapted to perform automated experiments by the use of an xyz-stage.
GDOES (glow discharge optical emission spectroscopy)
Instrument: GDA 750 (Spectruma Analytik) / Automated up to 24 samples
This technique provides a rapid and direct element analysis and depth profiling of solids (metals, powders, polymers, etc…).
Using GDOES, material layers are removed from the surface by the creation of a plasma. This plasma is responsible for the cathodic sputtering. The atoms removed are than migrated to the plasma where they are excited through collisions with electrons. The spectrum emitted by this collision is measured by a spectrometer and allows identification of the atoms, and subsequently of the surface of the material. Depending on the experimentation time different layers can be removed and analyzed.
Surface energy by drop shape analysis.
Instrument: FTA 2000 (First Ten Angstrom) / automated up to 24 samples
The instrument at Flamac uses the drop shape analysis method. This is a well respected and convenient way to measure contact angles and thereby determine surface energy. Contact angles are measured by fitting a mathematical expression to the shape of the drop and then calculating the slope of the tangent to the drop at the liquid-solid-vapor (LSV) interface line.
Using an xyz- stage this instrument can perform automated measurements. The following measurement modes are available:
- Static sessile drop method (contact angle at equilibrium)
- Dynamic sessile drop method: The volume of the droplet is increased during the measurement. (contact angle at non-equilibrium)
- Tilted plate experiments: A droplet is placed on a surface and afterwards the surface is tilted in a controlled way. The advancing and receding angle are monitored.
Instrument: Nicolet 6700 (Thermo) / automated up to 24 samples
Similar to all spectroscopic techniques, FT-IR can be used to identify compounds or investigate sample composition. Infrared spectroscopy correlation tables are tabulated in the literature.
Fourier transform infrared (FT-IR) spectroscopy is a measurement technique for collecting infrared spectra. Instead of recording the amount of energy absorbed when the frequency of the infra-red light is varied (monochromator), the IR light is guided through an interferometer. After passing through the sample, the measured signal is the interferogram. Performing a Fourier transform on this signal data results in a spectrum identical to that from conventional (dispersive) infrared spectroscopy.
Instrument:UNET (ASMEC) / automated up to 24 samples
Indentation (macro or micro) is one of the most applied means of testing the mechanical properties of materials, giving information on the scratch resistance, hardness, stiffness and elasticity. Nano-indentation is used to determine the indentation properties of material surfaces using a very hard and small tip (mostly diamond). This allows more precise and direct measurements from a nano up to a micro scale.
The instrument at FLAMAC is equipped with a confocal microscope to image the indented surface in order to detect scratch resistance, pile up, … . Imaging analysis can be applied afterwards.
Instrument: Phys Tech
This automated setup was co-developed by Flamac and is capable of measuring the electrical conductivity / resistivity of thin films using Van der Pauw method (measurement of the Hall Effect).
High-throughput Gas chromatography
Instrument: Trace GC ultra (Thermo) / Automated up to 192 samples
Gas chromatography (GC), is a common type of chromatography used in analytic chemistry for separating and analyzing compounds that can be vaporized without decomposition. Typical uses of GC include testing the purity of a particular substance, or separating the different components of a mixture (the relative amounts of such components can also be determined). In some situations, GC may help in identifying a compound. In preparative chromatography, GC can be used to prepare pure compounds from a mixture.
Instrument: ASC (Anton Paar) / Automated up to 32 samples
Rheology is the study of the flow of matter (liquids, soft solids) under stress. Flowing and elastic deformation behaviour are recorded. It applies to substances which have a complex structure, including formulations, sludges, suspensions, polymers, food additives, etc… The flow of these substances cannot be characterized by a single value of viscosity (at a fixed temperature and fixed shear rate) – instead the structure is recorded in function of changing conditions (shear, deformation, temperature)
The following properties can be characterized by rheological measurements:
- viscosity in function of shear
- stability of emulsions / suspensions
- shear thickening / shear thinning behavior
- processing ability
- yield point
The instrument available at Flamac can measure the rheological properties of liquids in an automated fashion. Automated cleaning and drying cycles are included. More information about the instrument can be found on the website of Anton Paar.
Applications: Coatings / Household products / Inks / Resins / Polymer solutions / lotions / Emulsions / Suspensions / …