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  • IµS & Scatex for (GI)SAXS
  • In-situ GISAXS for Liquids and Thin Films
  • Small Angle Scattering with METALJET
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Montel Optics

SAXS setup with a typical 3-pinhole collimation system
The illustration clearly shows that even with an antiscatter pinhole the beam stop needs a large diameter due to the parasitic aperture scattering. Using SCATEX pinholes instead, the scatter guard becomes dispensable and the minimum beam stop diameter decreases. Thus, SCATEX pinholes enable a higher resolution and photon flux.

Scattering intensity of a rat tail tendon measured with a 3-pinhole high-resolution NANOSTAR and a modified 2-pinhole NANOSTAR equipped with SCATEX pinholes
The resolution of both setups is very similar, but the setup with SCATEX pinholes gives a significantly higher scattering intensity.

IμS and SCATEX upgrade on a customized SAXS setup in Hamburg, Germany

Bruker NANOSTAR in Vienna, Austria

Huber system for SAXS in Tamkang, Taiwan

Results of a Mo/Si multilayer measured with the NANOSTAR and the synchrotron beamline BW4 at the Hasylab
Both measurements clearly show three Bragg sheets. In comparison the NANOSTAR results have a higher background and thus a lower resolution.

IµS and SCATEX for GI(SAXS)

Small-Angle X-ray Scattering - The Universe of Nanostructure Analysis

Today, the most exciting advances in new industrial materials and processes are based on key technologies in the nanoscale-domain (10-9m). Pharmaceuticals, cosmetics, functional food, smart polymers, intelligent surface coatings, sensorics and diagnostics greatly benefit from the tremendous process in nanoscience.

The ability to visualize structures being formed is the critical success factor in nanoscience and nanotechnology, in particular since visible light microscopy fails to provide information in this scale. SAXS and GISAXS are the most powerful ‘nanoscopical’ tools in this pursuit, yielding information in the range from 1 nm to above 0.1. µm, not only on nanoparticle sizes, shape and size distributions, but also on structural dynamics from a large variety of materials, such as liquid crystals, surface characteristics, powders, bulk samples, and thin films.

SAXS in combination with protein crystallography (PX) and Nuclear Magnetic Resonance (NMR) play an important role in offering a more complete view on complex biological nanosystems. For instance, most of today’s studies on proteins, membranes or large bio-functional complexes already use this powerful ‘hybrid analytical approach’, whereby SAXS provides essential constraints on particle shape and size for high-resolution modeling of NMR and PX data.

Incoatecs microfocus source IµS is part of Brukers comprehensive series of solutions for SAXS and GISAXS. In the newest NANOSTAR and N8 Horizon Incoatecs scatterless pinholes SCATEX are also integrated for higher performance, smaller footprint and better results.

Adaptation to UHV deposition chamber for in-situ GISAXS studies in Bratislava, Slovakia

In-situ GISAXS with liquid samples
For rapid GISAXS measurements of liquid samples our IµS was combined with a Dectris Pilatus detector. Silver particles on a Langmuir film were analyzed at different surface pressures which were applied by means of a reduction of the surface area. It was possible to study the formation process from unordered islands to ordered layers by increasing the pressure on the surface.

Measurement details:
- angle of incidence: 0.2deg
- measurement time: 180 sec
- aperture 350 µm
- the surface was pressed with 0 up to 26 mN/m

Unpressed surface 0 nm/m:
islands of nanoparticles are swimming on the surface without connection
Increased surface pressure 16 - 26 nm/m:
intensity increases, islands coalescence
at 26 mN/m “crystal“ peaks appear, vertical formation of hexagonal layers

In-situ GISAXS during Thin Film Growth

With the method of grazing incidence small angle scattering GISAXS a reliable and simple monitor of nanoparticle arrangement is available. Due to the development of high-brilliance microfocus sources like the IµS, there are now enough photons produced to measure GISAXS signals not only at synchrotrons, but also in the lab during the evolution of ordering in the nanometer range. At the Slovak Academy of Science in Bratislava, one of our customers shows that it is possible to measure nanoparticle ordering phenomena on a liquid surface also dynamically. In a second set-up, they use the IµS for in-situ GISAXS during film growth by ion beam sputtering. First experiments were done during the production of multilayer mirrors and the deposition of metals on graphene. For more information, please take a look into the download section.

Working principle of the METALJET X-ray source

SAXS scattering plot and radial integration of a Ag Behenate sample, measured with a Bruker AXS NANOSTAR equipped with the METALJET X-ray source

SAXS scattering plot of a very thin fiber from a rat tail tendon, measured with a Bruker AXS NANOSTAR equipped with the METALJET X-ray source

Small Angle Scattering with METALJET

The unprecedented brightness of the METALJET X-ray source now enables researchers to perform demanding experiments in their home-lab that previously could only be accomplished at a synchrotron. For high-resolution small angle scattering experiments, we have developed a superb synchrotron-type multilayer optics that enables 3 times more flux than modern microfocus rotating anodes in a very parallel beam with a divergence of below 0.5 mrad. Even more, the intensity of such a small angle scattering setup can be further increased by a factor of about 2.5 when using our scatter-free SCATEX pinholes.

The METALJET enables structural biologists, as well as material scientists to collect data on the most challenging samples, improving their home-lab productivity more than ever before.

 

 

Scientific Posters about (GI)SAXS

Applications with the Incoatec Microfocus Source IμS

System Upgrades with Incoatec´s Unique Microfocus Source and Scatterless Pinholes

GISAXS with Nanoparticles on Liquids and with Multilayer Films on a Lab Source

The Incoatec Microfocus Source for XRD-Applications

Trends on Multilayer X-ray Optics and Scatterless Apertures for X-ray Analytical Equipment

Improvement of SAXS Lab Equipment by Using Scatterless Apertures

 

Publications of Customers

1) Nanoparticles on a liquid sample were investigated with a special GISAXS setup equipped with a Cu-IµS producing a 5 mrad focused beam and with a Pilatus pixel detector. Ordering phenomena could be observed in-situ during an increase of surface pressure. The particles were transformed from single islands to an almost vertically ordered structure of connecting particles. PDF Download here.

2) By using in-situ GISAXS in the home-lab it was investigated how a multilayer grows during thin film deposition. This kind of experiments is typically done only at synchrotrons. With an IµS it is now also feasible in the home-lab.
See publication: "In-situ GISAXS monitoring of ultrashort period W/B4C multilayer x-ray mirror growth" by Martin Hodas, Peter Siffalovic et al  from the Slovak Academy of Science, Bratislava; Proc. SPIE 9588, Advances in X-Ray/EUV Optics and Components X, 958804 (2015); doi:10.1117/12.2187999

3) The publication  "Real-time SAXS study of a strain gauge based on a self-assembled goldnanoparticle monolayer" by Karol Vegso et al. shows some metal-jet X-ray source applications for SAXS, GISAXS, small-angle diffraction with an collimating Montel optics. The SAXS setup was equipped with a double-pinhole collimator made of scaterless pinholes Scatex of 550 m diameter; DOI:10.1016/j.sna.2016.02.021