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Advanced grazing-incidence techniques for modern soft-matter materials analysis.

Hexemer A, Müller-Buschbaum P - IUCrJ (2015)

Bottom Line: The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques.Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies.In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

View Article: PubMed Central - HTML - PubMed

Affiliation: Advanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720, USA.

ABSTRACT
The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities for in situ and in operando GISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

No MeSH data available.


Related in: MedlinePlus

(a) GISAXS setup with a microfluidic cell. The incoming X-ray beam with incident angle αi is depicted in red. The scattered intensity, with exit angle αf and out-of-plane angle Ψ, is recorded on a two-dimensional detector. (b) An illustration of the X-ray beam transmitted through the channel walls and its footprint on the sample surface. Note that, for clarity, the incident angle and the X-ray beam are not to scale. (c) A composite image of vertical line profiles at qy = 0 for 210 consecutive measurements scanning the microfluidic channel along the y direction while gold nanoparticles attach to a poly(ethyleneimine) thin film. Regions in black correspond to the position of the specular beamstop and the inter-module gaps of the Pilatus detector. Numbers indicate the different regimes in the microfluidic experiment. (d) Horizontal line profiles for an in situ microfluidic experiment as the sum of ten consecutive measurements. For clarity, the intensity is shifted along the intensity axis, with the initially dry film at the bottom. Reprinted with permission from Santoro et al. (2014 ▶). Copyright (2014) AIP Publishing.
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fig5: (a) GISAXS setup with a microfluidic cell. The incoming X-ray beam with incident angle αi is depicted in red. The scattered intensity, with exit angle αf and out-of-plane angle Ψ, is recorded on a two-dimensional detector. (b) An illustration of the X-ray beam transmitted through the channel walls and its footprint on the sample surface. Note that, for clarity, the incident angle and the X-ray beam are not to scale. (c) A composite image of vertical line profiles at qy = 0 for 210 consecutive measurements scanning the microfluidic channel along the y direction while gold nanoparticles attach to a poly(ethyleneimine) thin film. Regions in black correspond to the position of the specular beamstop and the inter-module gaps of the Pilatus detector. Numbers indicate the different regimes in the microfluidic experiment. (d) Horizontal line profiles for an in situ microfluidic experiment as the sum of ten consecutive measurements. For clarity, the intensity is shifted along the intensity axis, with the initially dry film at the bottom. Reprinted with permission from Santoro et al. (2014 ▶). Copyright (2014) AIP Publishing.

Mentions: The use of a moderately microfocused X-ray beam allows for new perspectives in GISAXS, since smaller samples can be investigated. The advantage of using small beams becomes apparent if sample preparation on a square-centimeter scale is challenging, or for samples in a complex sample environment. As an example for a complex sample environment, a combination of GISAXS with a microfluidic cell shows the great potential of this approach (Körstgens et al., 2014 ▶; Santoro et al., 2014 ▶). GISAXS at the solid–liquid interface typically suffers from the high absorption of the X-ray beam in the liquid phase in the common energy range for hard X-rays. With the use of a microfluidic device instead of a liquid cell, the X-ray beam path inside the liquid is significantly reduced, which allows for the use of the common X-ray energies available at beamlines typically used for GISAXS (Moulin et al., 2008 ▶). Of course, the sample area inside the microfluidic cell is strongly reduced compared with a liquid cell as well, which would also result in over-illumination using a large X-ray beam. Fig. 5 ▶ shows an example using GISAXS in combination with a microfluidic cell (Santoro et al., 2014 ▶). The attachment of gold nanoparticles to a poly(ethyleneimine) film surface from the flow of a gold nanoparticle solution through the microfluidic channel was monitored. Figs. 5 ▶(a) and 5 ▶(b) illustrate the scattering geometry and the combination of GISAXS and the microfluidic cell. Consecutive GISAXS measurements were performed by scanning the microfluidic channel along the y direction while gold nanoparticles were adsorbed at the surface. Due to the large number of collected two-dimensional GISAXS data, plotting all the two-dimensional GISAXS patterns or all corresponding line cuts from the two-dimensional GISAXS data is not meaningful. Instead, the use of so-called mappings has been established to help visualize the data better. Fig. 5 ▶(c) shows such a mapping composed of vertical line cuts from the two-dimensional GISAXS data, plotted as a function of time. In such a representation, changes are easily observed. However, the analysis is performed on complete two-dimensional GISAXS data or the line cuts. Fig. 5 ▶(d) shows a selection of horizontal line cuts to demonstrate the clear changes in the scattering data arising from lateral structures (Santoro et al., 2014 ▶).


Advanced grazing-incidence techniques for modern soft-matter materials analysis.

Hexemer A, Müller-Buschbaum P - IUCrJ (2015)

(a) GISAXS setup with a microfluidic cell. The incoming X-ray beam with incident angle αi is depicted in red. The scattered intensity, with exit angle αf and out-of-plane angle Ψ, is recorded on a two-dimensional detector. (b) An illustration of the X-ray beam transmitted through the channel walls and its footprint on the sample surface. Note that, for clarity, the incident angle and the X-ray beam are not to scale. (c) A composite image of vertical line profiles at qy = 0 for 210 consecutive measurements scanning the microfluidic channel along the y direction while gold nanoparticles attach to a poly(ethyleneimine) thin film. Regions in black correspond to the position of the specular beamstop and the inter-module gaps of the Pilatus detector. Numbers indicate the different regimes in the microfluidic experiment. (d) Horizontal line profiles for an in situ microfluidic experiment as the sum of ten consecutive measurements. For clarity, the intensity is shifted along the intensity axis, with the initially dry film at the bottom. Reprinted with permission from Santoro et al. (2014 ▶). Copyright (2014) AIP Publishing.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4285885&req=5

fig5: (a) GISAXS setup with a microfluidic cell. The incoming X-ray beam with incident angle αi is depicted in red. The scattered intensity, with exit angle αf and out-of-plane angle Ψ, is recorded on a two-dimensional detector. (b) An illustration of the X-ray beam transmitted through the channel walls and its footprint on the sample surface. Note that, for clarity, the incident angle and the X-ray beam are not to scale. (c) A composite image of vertical line profiles at qy = 0 for 210 consecutive measurements scanning the microfluidic channel along the y direction while gold nanoparticles attach to a poly(ethyleneimine) thin film. Regions in black correspond to the position of the specular beamstop and the inter-module gaps of the Pilatus detector. Numbers indicate the different regimes in the microfluidic experiment. (d) Horizontal line profiles for an in situ microfluidic experiment as the sum of ten consecutive measurements. For clarity, the intensity is shifted along the intensity axis, with the initially dry film at the bottom. Reprinted with permission from Santoro et al. (2014 ▶). Copyright (2014) AIP Publishing.
Mentions: The use of a moderately microfocused X-ray beam allows for new perspectives in GISAXS, since smaller samples can be investigated. The advantage of using small beams becomes apparent if sample preparation on a square-centimeter scale is challenging, or for samples in a complex sample environment. As an example for a complex sample environment, a combination of GISAXS with a microfluidic cell shows the great potential of this approach (Körstgens et al., 2014 ▶; Santoro et al., 2014 ▶). GISAXS at the solid–liquid interface typically suffers from the high absorption of the X-ray beam in the liquid phase in the common energy range for hard X-rays. With the use of a microfluidic device instead of a liquid cell, the X-ray beam path inside the liquid is significantly reduced, which allows for the use of the common X-ray energies available at beamlines typically used for GISAXS (Moulin et al., 2008 ▶). Of course, the sample area inside the microfluidic cell is strongly reduced compared with a liquid cell as well, which would also result in over-illumination using a large X-ray beam. Fig. 5 ▶ shows an example using GISAXS in combination with a microfluidic cell (Santoro et al., 2014 ▶). The attachment of gold nanoparticles to a poly(ethyleneimine) film surface from the flow of a gold nanoparticle solution through the microfluidic channel was monitored. Figs. 5 ▶(a) and 5 ▶(b) illustrate the scattering geometry and the combination of GISAXS and the microfluidic cell. Consecutive GISAXS measurements were performed by scanning the microfluidic channel along the y direction while gold nanoparticles were adsorbed at the surface. Due to the large number of collected two-dimensional GISAXS data, plotting all the two-dimensional GISAXS patterns or all corresponding line cuts from the two-dimensional GISAXS data is not meaningful. Instead, the use of so-called mappings has been established to help visualize the data better. Fig. 5 ▶(c) shows such a mapping composed of vertical line cuts from the two-dimensional GISAXS data, plotted as a function of time. In such a representation, changes are easily observed. However, the analysis is performed on complete two-dimensional GISAXS data or the line cuts. Fig. 5 ▶(d) shows a selection of horizontal line cuts to demonstrate the clear changes in the scattering data arising from lateral structures (Santoro et al., 2014 ▶).

Bottom Line: The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques.Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies.In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

View Article: PubMed Central - HTML - PubMed

Affiliation: Advanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720, USA.

ABSTRACT
The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities for in situ and in operando GISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.

No MeSH data available.


Related in: MedlinePlus