Raw data for "X-ray studies bridge the molecular and macro length scales during the emergence of CoO assemblies"

Raw data for „X-ray studies bridge the molecular and macro length scales during the emergence of CoO assemblies“

TEM and SEM

• SEM image of CoO assemblies after 90 min
• TEM images of CoO assemblies after 5, 10, 15, 20, 40, 60 and 90 min
• HR-TEM images of CoO assemblies after 90 min
• ED patterns of CoO assemblies after 10, 15 and 20 min

HERFD-XANES

In situ spectra for the CoO synthesis at 160°C were recorded at beamline ID26 at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. Using a Si (111) double crystal monochromator, the incident energy was varied from 7.70 to 7.78 keV. The emitted fluorescence was measured with an emission spectrometer in Rowland geometry with five Si (531) analyzer crystals aligned at the Bragg angle of 77°. HERFD-XANES spectra were recorded in continuous scan mode every 80 s with average energy steps of 0.05 eV. The data set consists of one file containing a sequential set of energy scans, representing the pre- and main edge regions of the HERFD-XANES spectra.

Important column identifiers:

• incident energy: “arr_hdh_ene”
• incident intensity: “I02”
• fluorescence intensity: “apd”

X-ray total scattering

Data was taken at beamline P21.1 of PETRA III at Deutsches Elektronen-Synchrotron (DESY), Hamburg, Germany. Diffraction patterns were recorded every 10 s at an X-ray energy of 102.92 keV (λ = 0.121 Å) with an XRD1621 detector (Perkin Elmer Inc., USA) with a pixel size of 200 × 200 μm² and a sample-to-detector distance of 0.411 m. The dataset consist of

• in situ data set of CoO nanoassembly synthesis at 160°C
• in situ data set of CoO nanoassembly synthesis at 140°C
• ex situ samples prepared at 160 °C at different times
• commercial reference compounds in powder and 0.1 M BnOH solution

data format: 2D scattering patterns in .tif format

The total scattering data is split into individual archives for the above subsets.

SAXS and PXRD

data set “laboratory_SAXS_data”:

Data were recorded with the laboratory molybdenum anode microfocus X-ray setup at LMU, Munich. SAXS data are multiple successive 20 min exposures. Transmission data are 10 s exposures with the beamstop removed.

data format: .tif detector images recorded with a Dectris Pilatus 300K.
X-ray wavelength: 0.71075 Angstrom
Calibrant for sample-to-detector distance, beam center and detector tilt: Silver behenate (AgBeh)

data set “synchrotron_SAXS_data”:

Data were recorded at beamline P03 at PETRA III, DESY, Hamburg. Data are recorded separately at a long and a short sample-to-detector distance. At the long distance, the exposure time is 5x0.1s. At the short distance, the exposure time is 1x0.5s.

data format: .cbf detector images recorded with a Dectris Pilatus 1M.
X-ray wavelength: 0.961 Angstrom
Calibrant for sample-to-detector distance, beam center and detector tilt: Silver behenate (AgBeh) 

data set “laboratory_PXRD_data”:

Data were recorded with the laboratory molybdenum anode microfocus X-ray setup at LMU, Munich. The overlap for stitching is 10 px in both horizontal and vertical direction.

The recording sequence is
01 02 07
03 04 08
05 06 09
10 11 12
13 14 15
with 3 images at each position, to take the median. The exposure time per image is 1200 s.

For LaB6 the sequence is
01 02
03 04
05 06
07 08
09 10
with 5 images at each position, to take the median. The exposure time per image is 300 s.

data format: .tif detector images recorded with a Dectris Pilatus 100K.
X-ray wavelength: 0.71 Angstrom
Calibrant for sample-to-detector distance, beam center and detector tilt: Lanthanum hexaboride NIST SRM 660c (LaB6)