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Scanning force microscope for in situ nanofocused X-ray diffraction studies.

Ren Z, Mastropietro F, Davydok A, Langlais S, Richard MI, Furter JJ, Thomas O, Dupraz M, Verdier M, Beutier G, Boesecke P, Cornelius TW - J Synchrotron Radiat (2014)

Bottom Line: Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate.The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area.This in situ approach gives access to the mechanical behavior of nanomaterials.

View Article: PubMed Central - HTML - PubMed

Affiliation: IM2NP (UMR 7334), Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen - Case 142, F-13397 Marseille, France.

ABSTRACT
A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials.

No MeSH data available.


Schematic of the experimental set-up at the ID01 beamline at ESRF in Grenoble (France). (1) Synchrotron, (2) double-bounce channel-cut Si111 monochromator, (3) high-precision slits, (4) Fresnel zone plate, (5) order-sorting aperture, (6) SFINX, (7) detector: MAXIPIX or APD.
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fig2: Schematic of the experimental set-up at the ID01 beamline at ESRF in Grenoble (France). (1) Synchrotron, (2) double-bounce channel-cut Si111 monochromator, (3) high-precision slits, (4) Fresnel zone plate, (5) order-sorting aperture, (6) SFINX, (7) detector: MAXIPIX or APD.

Mentions: The new tool was installed on the diffractometer at the ID01 beamline at ESRF in Grenoble (France). The experimental set-up is schematically depicted in Fig. 2 ▸. During this experiment the X-ray beam was monochromated to an energy of 8.97 keV (λ = 0.138 nm) using the double-bounce channel-cut Si111 monochromator [(2) in Fig. 2 ▸]. The monochromator has a bandwidth of 10−4 which translates to a longitudinal coherence length of 1.4 µm. By means of a tungsten Fresnel zone plate (FZP) with a diameter of 300 µm and an outer zone width of 80 nm which was mounted in air, the monochromatic beam was focused down to 400 nm vertically (V) and 900 nm horizontally (H). The beam size was determined by a knife-edge scan employing a tungsten wire with diameter of 200 µm [(4) in Fig. 2 ▸]. An order-sorting aperture [(5) in Fig. 2 ▸] with a diameter of 50 µm was installed 2.5 cm upstream from the sample for selecting the first diffraction order of the FZP. High-precision slits [(3) in Fig. 2 ▸] were installed right in front of the FZP. For coherent X-ray diffraction studies, they were closed to match the transverse coherence lengths of the beamline amounting to approximately 20 and 60 µm in the horizontal and vertical direction, respectively. The diffractometer allows for rotating SFINX into the Bragg condition while keeping the AFM-tip always vertical with respect to the sample surface [(6) in Fig. 2 ▸]. When installed on a marble table in a standard laboratory in Marseille the peak-to-peak noise of SFINX amounts to ∼5 nm increasing to about 15 nm when being installed on the diffractometer. The difference in noise is attributed to the comparatively harsh environment at a synchrotron beamline where mechanical vacuum pumps run continuously and where the device is installed on a rotatable support of the diffractometer being less rigid than a marble table. The diffracted X-ray beam was recorded either by a two-dimensional MAXIPIX pixel detector with a pixel size of 55 µm × 55 µm or a point detector, i.e. an avalanche photodiode (APD) [(7) in Fig. 2 ▸]. Both detectors were mounted 1.27 m downstream from the sample position.


Scanning force microscope for in situ nanofocused X-ray diffraction studies.

Ren Z, Mastropietro F, Davydok A, Langlais S, Richard MI, Furter JJ, Thomas O, Dupraz M, Verdier M, Beutier G, Boesecke P, Cornelius TW - J Synchrotron Radiat (2014)

Schematic of the experimental set-up at the ID01 beamline at ESRF in Grenoble (France). (1) Synchrotron, (2) double-bounce channel-cut Si111 monochromator, (3) high-precision slits, (4) Fresnel zone plate, (5) order-sorting aperture, (6) SFINX, (7) detector: MAXIPIX or APD.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4862253&req=5

fig2: Schematic of the experimental set-up at the ID01 beamline at ESRF in Grenoble (France). (1) Synchrotron, (2) double-bounce channel-cut Si111 monochromator, (3) high-precision slits, (4) Fresnel zone plate, (5) order-sorting aperture, (6) SFINX, (7) detector: MAXIPIX or APD.
Mentions: The new tool was installed on the diffractometer at the ID01 beamline at ESRF in Grenoble (France). The experimental set-up is schematically depicted in Fig. 2 ▸. During this experiment the X-ray beam was monochromated to an energy of 8.97 keV (λ = 0.138 nm) using the double-bounce channel-cut Si111 monochromator [(2) in Fig. 2 ▸]. The monochromator has a bandwidth of 10−4 which translates to a longitudinal coherence length of 1.4 µm. By means of a tungsten Fresnel zone plate (FZP) with a diameter of 300 µm and an outer zone width of 80 nm which was mounted in air, the monochromatic beam was focused down to 400 nm vertically (V) and 900 nm horizontally (H). The beam size was determined by a knife-edge scan employing a tungsten wire with diameter of 200 µm [(4) in Fig. 2 ▸]. An order-sorting aperture [(5) in Fig. 2 ▸] with a diameter of 50 µm was installed 2.5 cm upstream from the sample for selecting the first diffraction order of the FZP. High-precision slits [(3) in Fig. 2 ▸] were installed right in front of the FZP. For coherent X-ray diffraction studies, they were closed to match the transverse coherence lengths of the beamline amounting to approximately 20 and 60 µm in the horizontal and vertical direction, respectively. The diffractometer allows for rotating SFINX into the Bragg condition while keeping the AFM-tip always vertical with respect to the sample surface [(6) in Fig. 2 ▸]. When installed on a marble table in a standard laboratory in Marseille the peak-to-peak noise of SFINX amounts to ∼5 nm increasing to about 15 nm when being installed on the diffractometer. The difference in noise is attributed to the comparatively harsh environment at a synchrotron beamline where mechanical vacuum pumps run continuously and where the device is installed on a rotatable support of the diffractometer being less rigid than a marble table. The diffracted X-ray beam was recorded either by a two-dimensional MAXIPIX pixel detector with a pixel size of 55 µm × 55 µm or a point detector, i.e. an avalanche photodiode (APD) [(7) in Fig. 2 ▸]. Both detectors were mounted 1.27 m downstream from the sample position.

Bottom Line: Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate.The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area.This in situ approach gives access to the mechanical behavior of nanomaterials.

View Article: PubMed Central - HTML - PubMed

Affiliation: IM2NP (UMR 7334), Aix-Marseille Université, CNRS, Faculté des Sciences, Campus de Saint-Jérôme, Avenue Escadrille Normandie Niemen - Case 142, F-13397 Marseille, France.

ABSTRACT
A compact scanning force microscope has been developed for in situ combination with nanofocused X-ray diffraction techniques at third-generation synchrotron beamlines. Its capabilities are demonstrated on Au nano-islands grown on a sapphire substrate. The new in situ device allows for in situ imaging the sample topography and the crystallinity by recording simultaneously an atomic force microscope (AFM) image and a scanning X-ray diffraction map of the same area. Moreover, a selected Au island can be mechanically deformed using the AFM tip while monitoring the deformation of the atomic lattice by nanofocused X-ray diffraction. This in situ approach gives access to the mechanical behavior of nanomaterials.

No MeSH data available.