scholarly journals Does 1,8-diiodooctane affect the aggregation state of PC 71 BM in solution?

2018 ◽  
Vol 5 (9) ◽  
pp. 180937 ◽  
Author(s):  
Gabriel Bernardo ◽  
Adam. L. Washington ◽  
Yiwei Zhang ◽  
Stephen. M. King ◽  
Daniel. T. W. Toolan ◽  
...  
Keyword(s):  
Small Angle ◽  
Acid Methyl Ester ◽  
X Rays ◽  
Aggregation State ◽  
Solar Cell Performance ◽  
X Ray ◽  
X Ray Scattering ◽  
High Boiling Solvent ◽  
Film Thinning ◽  
Induced Aggregation

1,8-Diiodooctane (DIO) is an additive used in the processing of organic photovoltaics and has previously been reported, on the basis of small-angle X-ray scattering (SAXS) measurements, to deflocculate nano-aggregates of [6,6]-phenyl-C71-butyric acid methyl ester (PC 71 BM) in chlorobenzene. We have critically re-examined this finding in a series of scattering measurements using both X-rays and neutrons. With SAXS, we find that the form of the background solvent scattering is influenced by the presence of DIO, that there is substantial attenuation of the X-rays by the background solvent and that there appears to be beam-induced aggregation. All three factors call into question the suitability of SAXS for measurements on these samples. By contrast, small-angle neutron scattering (SANS) measurements, performed at concentrations of 15 mg ml −1 up to and including 40 mg ml −1 , show no difference in the aggregation state for PC 71 BM in chlorobenzene with and without 3% DIO; we find PC 71 BM to be molecularly dissolved in all solvent cases. In situ film thinning measurements of spin-coated PC 71 BM solution with the DIO additive dry much slower. Optical imaging shows that the fullerene films possess enhanced molecular mobility in the presence of DIO and it is this which, we conclude, improves the nanomorphology and consequently solar cell performance. We propose that any compatible high boiling solvent would be expected to show the same behaviour.

scholarly journals Combined scanning small-angle X-ray scattering and holography probes multiple length scales in cell nuclei

2021 ◽  
Vol 28 (2) ◽  
pp. 518-529
Author(s):  
Andrew Wittmeier ◽  
Chiara Cassini ◽  
Mareike Töpperwien ◽  
Manuela Denz ◽  
Johannes Hagemann ◽  
...  
Keyword(s):  
Small Angle ◽  
Nuclear Material ◽  
X Rays ◽  
Cell Nuclei ◽  
Aggregation State ◽  
Intact Cells ◽  
Length Scales ◽  
X Ray ◽  
X Ray Scattering ◽  
Ray Scattering

X-rays are emerging as a complementary probe to visible-light photons and electrons for imaging biological cells. By exploiting their small wavelength and high penetration depth, it is possible to image whole, intact cells and resolve subcellular structures at nanometer resolution. A variety of X-ray methods for cell imaging have been devised for probing different properties of biological matter, opening up various opportunities for fully exploiting different views of the same sample. Here, a combined approach is employed to study cell nuclei of NIH-3T3 fibroblasts. Scanning small-angle X-ray scattering is combined with X-ray holography to quantify length scales, aggregation state, and projected electron and mass densities of the nuclear material. Only by joining all this information is it possible to spatially localize nucleoli, heterochromatin and euchromatin, and physically characterize them. It is thus shown that for complex biological systems, like the cell nucleus, combined imaging approaches are highly valuable.

A Small-Angle X-Ray Scattering Study on Pre-Irradiated Malate Synthase. The Influence of Formate, Superoxide Dismutase, and Catalase on the X-Ray Induced Aggregation of the Enzyme

1985 ◽  
Vol 40 (5-6) ◽  
pp. 364-372 ◽  
Author(s):  
P. Zipper ◽  
R. Wilfing ◽  
M. Kriechbaum ◽  
H. Durchschlag
Keyword(s):  
Aqueous Solution ◽  
Superoxide Dismutase ◽  
Small Angle ◽  
Malate Synthase ◽  
X Ray ◽  
X Ray Scattering ◽  
X Irradiation ◽  
The Mean ◽  
Induced Aggregation ◽  
Ray Scattering

Abstract The sulfhydryl enzyme malate synthase from baker’s yeast was X-irradiated with 6 kGy in air-saturated aqueous solution (enzyme concentration: ≃ 10 mg/ml; volume: 120 μl), in the absence or presence of the specific scavengers formate, superoxide dismutase, and catalase. After X-irradiation, a small aliquot of the irradiated solutions was tested for enzymic activity while the main portion was investigated by means of small-angle X-ray scattering. Additionally, an unir­radiated sample without additives was investigated as a reference. Experiments yielded the fol­lowing results: 1. X-irradiation in the absence of the mentioned scavengers caused considerable aggregation, fragmentation, and inactivation of the enzyme. The dose Dt37 for total (= repairable + non­-repayable) inactivation resulted as 4.4 kGy. The mean radius of gyration was found to be about 13 nm. The mean degree of aggregation was obtained as 5.7, without correction for fragmenta­tion. An estimation based on the thickness factor revealed that about 19% of material might be strongly fragmented. When this amount of fragments was accordingly taken into account, a value of 7.1 was obtained as an upper limit for the mean degree of aggregation. The observed retention of the thickness factor and the finding of two different cross-section factors are in full accord with the two-dimensional aggregation model established previously (Zipper and Durchschlag, Radiat. Environ. Biophys. 18, 99 - 121 (1980)). 2. The presence of catalytic amounts of superoxide dismutase and/or catalase, in the absence of formate, during X-irradiation reduced both aggregation and inactivation significantly. 3. The presence of formate (10 or 100 mᴍ) during X-irradiation led to a strong decrease of aggregation and inactivation. This effect was more pronounced with the higher formate concen­tration or when superoxide dismutase and/or catalase were simultaneously present during X-irradiation. The presence of formate also reduced the amount of fragments significantly. 4. The results clearly show that the aggregation and inactivation of malate synthase upon X-irradiation in aqueous solution are mainly caused by OH·; to a minor extent O·̄2 and H2O2 are additionally involved in the damaging processes.

A multi-length-scale USAXS/SAXS facility: 10–50 keV small-angle X-ray scattering instrument

2013 ◽  
Vol 46 (5) ◽  
pp. 1508-1512 ◽  
Author(s):  
Byron Freelon ◽  
Kamlesh Suthar ◽  
Jan Ilavsky
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
And Performance ◽  
New Facility ◽  
Ray Scattering

Coupling small-angle X-ray scattering (SAXS) and ultra-small-angle X-ray scattering (USAXS) provides a powerful system of techniques for determining the structural organization of nanostructured materials that exhibit a wide range of characteristic length scales. A new facility that combines high-energy (HE) SAXS and USAXS has been developed at the Advanced Photon Source (APS). The application of X-rays across a range of energies, from 10 to 50 keV, offers opportunities to probe structural behavior at the nano- and microscale. An X-ray setup that can characterize both soft matter or hard matter and high-Zsamples in the solid or solution forms is described. Recent upgrades to the Sector 15ID beamline allow an extension of the X-ray energy range and improved beam intensity. The function and performance of the dedicated USAXS/HE-SAXS ChemMatCARS-APS facility is described.

A new high-resolution small-angle X-ray scattering apparatus using a fine-focus rotating anode, point-focusing collimation and a position-sensitive proportional counter

1984 ◽  
Vol 17 (5) ◽  
pp. 337-343 ◽  
Author(s):  
O. Yoda
Keyword(s):  
High Resolution ◽  
Small Angle ◽  
Proportional Counter ◽  
Anisotropic Scattering ◽  
Photon Flux ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Position Sensitive ◽  
Ray Scattering

A high-resolution small-angle X-ray scattering camera has been built, which has the following features. (i) The point collimation optics employed allows the scattering cross section of the sample to be directly measured without corrections for desmearing. (ii) A small-angle resolution better than 0.5 mrad is achieved with a camera length of 1.6 m. (iii) A high photon flux of 0.9 photons μs−1 is obtained on the sample with the rotating-anode X-ray generator operated at 40 kV–30 mA. (iv) Incident X-rays are monochromated by a bent quartz crystal, which makes the determination of the incident X-ray intensity simple and unambiguous. (v) By rotation of the position-sensitive proportional counter around the direct beam, anisotropic scattering patterns can be observed without adjusting the sample. Details of the design and performance are presented with some applications.

Correlation of Small-Angle X-Ray Scattering and Solar Cell Performance of a-SiGe:H Alloys

1993 ◽  
Vol 297 ◽  
Author(s):  
S.J. Jones ◽  
Y. Chen ◽  
D.L. Williamson ◽  
X. Xu ◽  
J. Yang ◽  
...  
Keyword(s):  
Solar Cell ◽  
Small Angle ◽  
Film Surface ◽  
Nanometer Scale ◽  
Low Density ◽  
Solar Cell Performance ◽  
X Ray ◽  
X Ray Scattering ◽  
Cell Structures ◽  
Ray Scattering

Small-angle x-ray scattering (SAXS) measurements were made on a-SiGe:H alloys to study microstructure on the nanometer scale as a function of Ge content, and the results were compared with representative single-junction solar cell properties. Samples consisting of only the i-layer were used for SAXS. Above a Ge content of 20 %, a significant increase in SAXS was seen. From measurements made with the samples tilted relative to the incident x-ray beam, the increase in scattering is attributed to the appearance of elongated low density regions in the film, modeled as ellipsoidal microvoids, which are preferentially oriented perpendicular to the film surface and may be related to columnar-like microstructure. Flotation density measurements support the presence of low density regions. Initial and light-degraded measurements on corresponding solar cell structures do not show a correlation between SAXS and initial cell properties; there is, however, some evidence that the light-induced degradation is higher for cells with larger amounts of SAXS-detected microstructure and this needs further investigation.

Improved Signal-to-Background Ratio in Small-Angle X-ray Scattering Experiments with Synchrotron Radiation using an Evacuated Cell for Solutions

1997 ◽  
Vol 30 (1) ◽  
pp. 49-54 ◽  
Author(s):  
J.-M. Dubuisson ◽  
T. Decamps ◽  
P. Vachette
Keyword(s):  
Synchrotron Radiation ◽  
Small Angle ◽  
X Rays ◽  
X Ray ◽  
Tight Contact ◽  
X Ray Scattering ◽  
Quartz Capillary ◽  
Conventional Cell ◽  
Capillary Walls ◽  
Ray Scattering

An evacuated, temperature-controlled cell has been built for use on the small-angle X-ray scattering instrument D24 at the synchrotron radiation facility LURE. The sample is placed in a quartz capillary sealed in a stainless-steel holder using a vacuum-tight glue. Several O rings provide a vacuum path upstream and downstream from the cell, so that the X-ray beam only meets the capillary walls and the solution under study between the slits and the beam stop, while the sample is maintained under atmospheric pressure. The cell temperature is controlled via a water circulation through a copper sheath in tight contact with the steel holder. The use of this cell results in a marked reduction of the background, as observed in two series of parallel experiments using a conventional cell and this evacuated cell. The decrease ranges from a factor of 2 at s 1 values larger than 0.008 Å−1 to more than 15 at s = 0.00116 Å−1, where s is the modulus of the scattering vector (s = 2sin θ/λ, 2θ is the scattering angle and λ is the wavelength of the X-rays).

Apparatus for the simultaneous measurement of the X-ray absorption factor developed for a small-angle X-ray scattering beamline

2007 ◽  
Vol 40 (4) ◽  
pp. 791-795 ◽  
Author(s):  
Takeshi Morita ◽  
Yoshitada Tanaka ◽  
Kazuki Ito ◽  
Yoshihiro Takahashi ◽  
Keiko Nishikawa
Keyword(s):  
Small Angle ◽  
Performance Test ◽  
X Rays ◽  
Absorption Factor ◽  
X Ray ◽  
X Ray Scattering ◽  
X Ray Absorption ◽  
Scattering Measurement ◽  
Ray Scattering

A novel apparatus has been developed that enables the simultaneous determination of the absorption factor during measurement of small-angle X-ray scattering (SAXS) intensities of a sample. It was designed especially for the use of relatively low-energy X-rays at SAXS beamlines of synchrotron facilities. The X-ray intensity of transmittance is measured by a silicon PIN photodiode, which is implanted in a direct beamstop set in a vacuum chamber. Since the assembly transmits an attenuated direct beam to a detector during the scattering measurement, a zero-angle position can be monitored without additional operation. It was confirmed that the linearity between the signal from the photodiode and the intensity of X-rays is good and the photodiode is applicable for the desired purpose. For a performance test, the absorption factors of a supercritical fluid were measured with a wide density range.

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