skip to main content
US FlagAn official website of the United States government
dot gov icon
Official websites use .gov
A .gov website belongs to an official government organization in the United States.
https lock icon
Secure .gov websites use HTTPS
A lock ( lock ) or https:// means you've safely connected to the .gov website. Share sensitive information only on official, secure websites.

Explore Research Products in the PAR
It may take a few hours for recently added research products to appear in PAR search results.


Title: Observations of phase changes in monoolein during high viscous injection
Serial crystallography of membrane proteins often employs high-viscosity injectors (HVIs) to deliver micrometre-sized crystals to the X-ray beam. Typically, the carrier medium is a lipidic cubic phase (LCP) media, which can also be used to nucleate and grow the crystals. However, despite the fact that the LCP is widely used with HVIs, the potential impact of the injection process on the LCP structure has not been reported and hence is not yet well understood. The self-assembled structure of the LCP can be affected by pressure, dehydration and temperature changes, all of which occur during continuous flow injection. These changes to the LCP structure may in turn impact the results of X-ray diffraction measurements from membrane protein crystals. To investigate the influence of HVIs on the structure of the LCP we conducted a study of the phase changes in monoolein/water and monoolein/buffer mixtures during continuous flow injection, at both atmospheric pressure and under vacuum. The reservoir pressure in the HVI was tracked to determine if there is any correlation with the phase behaviour of the LCP. The results indicated that, even though the reservoir pressure underwent (at times) significant variation, this did not appear to correlate with observed phase changes in the sample stream or correspond to shifts in the LCP lattice parameter. During vacuum injection, there was a three-way coexistence of the gyroid cubic phase, diamond cubic phase and lamellar phase. During injection at atmospheric pressure, the coexistence of a cubic phase and lamellar phase in the monoolein/water mixtures was also observed. The degree to which the lamellar phase is formed was found to be strongly dependent on the co-flowing gas conditions used to stabilize the LCP stream. A combination of laboratory-based optical polarization microscopy and simulation studies was used to investigate these observations.  more » « less
Award ID(s):
1943448 1231306
PAR ID:
10400873
Author(s) / Creator(s):
; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; more » ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; « less
Date Published:
Journal Name:
Journal of Synchrotron Radiation
Volume:
29
Issue:
3
ISSN:
1600-5775
Page Range / eLocation ID:
602 to 614
Format(s):
Medium: X
Sponsoring Org:
National Science Foundation
More Like this
  1. ; ; ; ; ; ; ; ; ; ; et al (, Journal of Applied Crystallography)
    Serial femtosecond crystallography (SFX) is a powerful technique that exploits X-ray free-electron lasers to determine the structure of macromolecules at room temperature. Despite the impressive exposition of structural details with this novel crystallographic approach, the methods currently available to introduce crystals into the path of the X-ray beam sometimes exhibit serious drawbacks. Samples requiring liquid injection of crystal slurries consume large quantities of crystals (at times up to a gram of protein per data set), may not be compatible with vacuum configurations on beamlines or provide a high background due to additional sheathing liquids present during the injection. Proposed and characterized here is the use of an immiscible inert oil phase to supplement the flow of sample in a hybrid microfluidic 3D-printed co-flow device. Co-flow generation is reported with sample and oil phases flowing in parallel, resulting in stable injection conditions for two different resin materials experimentally. A numerical model is presented that adequately predicts these flow-rate conditions. The co-flow generating devices reduce crystal clogging effects, have the potential to conserve protein crystal samples up to 95% and will allow degradation-free light-induced time-resolved SFX. 
    more » « less
  2. ; ; ; ; ; ; ; ; ; (, Journal of Applied Physics)
    High-entropy alloys (HEAs) are a class of multi-element materials that exhibit unique structural and functional properties. This study reports on the synthesis and characterization of a superconducting HEA, (NbTa)0.55(HfTiZr)0.45 fabricated using the vacuum arc melting technique. Scanning electron microscopy and energy-dispersive x-ray spectroscopy were employed to analyze the material's morphology and composition. X-ray diffraction analysis revealed a single-phase body-centered cubic (BCC) structure with a measured nanoindentation hardness of 6.4 GPa and Young's modulus of 132 GPa. This HEA superconductor was investigated by x-ray diffraction at Beamline 13BM-C, Advanced Photon Source, and the BCC phase was stable to the highest pressure of 50 GPa. Superconductivity was characterized by four-probe resistivity measurements in a quantum design physical property measurement system, yielding a superconducting transition temperature (Tc) of 7.2 K at ambient pressure and reaching a maximum of 10.1 K at the highest applied pressure of 23.6 GPa. The combination of high structural stability enhanced superconducting performance under pressure and superior mechanical properties highlights (NbTa)0.55(HfTiZr)0.45 as a promising superconductor under extreme environments. 
    more » « less
  3. ; ; ; ; ; (, Soft Matter)
    Material relationships at low temperatures were determined for concentrated surfactant solutions using a combination of rheological experiments, cross-polarized microscopy, calorimetry, and small angle X-ray scattering. A lamellar structured 70 wt% solution of sodium laureth sulfate in water was used as a model system. At cold temperatures (5 °C and 10 °C), the formation of surfactant crystals resulted in extremely high viscosity. The bulk flow behavior of multi-lamellar vesicles (20 °C) and focal conic defects (90 °C) in the lamellar phase was similar. Shear-induced crystallization at temperatures higher than the equilibrium crystallization temperature range resulted in an unusual complex viscosity peak. The effects of processing-relevant parameters including temperature, cooling time, and applied shear were investigated. Knowledge of key low-temperature structure–property-processing relationships for concentrated feedstocks is essential for the sustainable design and manufacturing of surfactant-based consumer products for applications such as cold-water laundry. 
    more » « less
  4. ; ; ; ; (, Materials Advances)
    null (Ed.)
    A free-standing film composed of bilayered vanadium oxide nanoflakes is for the first time synthesized using a new low-energy process. The precursor powder, δ-Li x V 2 O 5 · n H 2 O, was prepared using a simple sol–gel based chemical preintercalation synthesis procedure. δ-Li x V 2 O 5 · n H 2 O was dispersed and probe sonicated in N -methyl pyrrolidone to exfoliate the bilayers followed by vacuum filtration resulting in the formation of a free-standing film with obsidian color. X-ray diffraction showed lamellar ordering of a single-phase material with a decreased interlayer distance compared to that of the precursor powder. Scanning electron microscopy images demonstrated stacking of the individual nanoflakes. This morphology was further confirmed with scanning transmission electron microscopy that showed highly malleable nanoflakes consisting of ∼10–100 vanadium oxide bilayers. One of the most important consequences of this morphological rearrangement is that the electronic conductivity of the free-standing film, measured by the four-probe method, increased by an order of magnitude compared to conductivity of the pressed pellet made of precursor powder. X-ray photoelectron spectroscopy measurements showed the coexistence of both V 5+ and V 4+ oxidation states in the exfoliated sample, possibly contributing to the change in electronic conductivity. The developed approach provides the ability to maintain the phase purity and crystallographic order during the exfoliation process, coupled with the formation of a free-standing film of enhanced conductivity. The produced bilayered vanadium oxide nanoflakes can be used as the building blocks for the synthesis of versatile two-dimensional heterostructures to create innovative electrodes for electrochemical energy storage applications. 
    more » « less
  5. ; ; ; ; ; (, Journal of Vacuum Science & Technology A)
    In the present study, thermal stability of α-Ga2O3 under vacuum and ambient pressure conditions was investigated in situ by x-ray diffraction and transmission electron microscopy (TEM). It was observed that the thermal stability of α-Ga2O3 increased by 200 °C when pressure was lowered from an atmospheric to a vacuum level. This finding can be explained by oxygen diffusion under different oxygen partial pressures. In addition, in situ TEM imaging revealed that, once past the decomposition temperature, the onset of phase change propagates from the top crystal surface and accumulates strain, eventually resulting in a fractural film. The mechanism of α-Ga2O3 to β-Ga2O3 transition is evaluated through experiments and is discussed in this manuscript. 
    more » « less
  • Citation Formats
  • MLA
  • APA
  • Chicago
  • BibTeX
  • Save / Share this Record
  • Send to Email