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1.
Rev Sci Instrum ; 94(11)2023 Nov 01.
Article in English | MEDLINE | ID: mdl-37938065

ABSTRACT

The horizontal time-of-flight neutron reflectometer at the reactor of the Delft University of Technology, The Netherlands, has been completely renewed, relocated, and upgraded and allows for the study of air/liquid, solid/liquid, and solid/air interfaces. Innovations in the redesign include (i) a completely flexible double disk chopper system allowing to choose the optimal wavelength resolution with exchangeable neutron guide sections between the chopper disks to increase intensity, (ii) a movable second diaphragm just before the sample position to better control the beam footprint on the sample and effectively decrease counting times, and (iii) guides along the entire flight path of the neutron reflectometer. The performance of the renewed reflectometer is illustrated with measurements of hydrogen sensing materials.

2.
Inorg Chem ; 62(18): 6981-6992, 2023 May 08.
Article in English | MEDLINE | ID: mdl-37120857

ABSTRACT

The quaternary compound Cs2Pb(MoO4)2 was synthesized and its structure was characterized using X-ray and neutron diffraction from 298 to 773 K, while thermal expansion was studied from 298 to 723 K. The crystal structure of the high-temperature phase ß-Cs2Pb(MoO4)2 was elucidated, and it was found to crystallize in the space group R3̅m (No. 166), i.e., with a palmierite structure. In addition, the oxidation state of Mo in the low-temperature phase α-Cs2Pb(MoO4)2 was studied using X-ray absorption near-edge structure spectroscopy. Phase diagram equilibrium measurements in the Cs2MoO4-PbMoO4 system were performed, revisiting a previously reported phase diagram. The equilibrium phase diagram proposed here includes a different composition of the intermediate compound in this system. The obtained data can serve as relevant information for thermodynamic modeling in view of the safety assessment of next-generation lead-cooled fast reactors.

3.
J Phys Chem C Nanomater Interfaces ; 125(30): 16391-16402, 2021 Aug 05.
Article in English | MEDLINE | ID: mdl-34386149

ABSTRACT

Iron is a promising, earth-abundant material for future energy applications. In this study, we use a neutron diffractometer to investigate the properties of an iron electrode in an alkaline environment. As neutrons penetrate deeply into materials, neutron scattering gives us a unique insight into what is happening inside the electrode. We made our measurements while the electrode was charging or discharging. Our key questions are: Which phases occur for the first and second discharge plateaus? And why are iron electrodes less responsive at higher discharge rates? We conclude that metallic iron and iron hydroxide form the redox pair for the first discharge plateau. For the second discharge plateau, we found a phase similar to feroxyhyte but with symmetrical and equally spaced arrangement of hydrogen atoms. The data suggest that no other iron oxide or iron (oxy)hydroxide formed. Remarkable findings include the following: (1) substantial amounts of iron hydroxide are always present inside the electrode. (2) Passivation is mostly caused by iron hydroxide that is unable to recharge. (3) Iron fractions change as expected, while iron hydroxide fractions are delayed, resulting in substantial amounts of amorphous, undetectable iron phases. About 40% of the participating iron of the first plateau and about 55% of the participating iron for the second plateau are undetectable. (4) Massive and unexpected precipitation of iron hydroxide occurs in the transition from discharging to charging. (2), (3), and (4) together cause accumulation of iron hydroxide inside the electrode.

4.
Phys Rev Lett ; 126(7): 070401, 2021 Feb 19.
Article in English | MEDLINE | ID: mdl-33666459

ABSTRACT

We have recently shown how a polarized beam in Talbot-Lau interferometric imaging can be used to analyze strong magnetic fields through the spin dependent differential phase effect at field gradients. While in that case an adiabatic spin coupling with the sample field is required, here we investigate a nonadiabatic coupling causing a spatial splitting of the neutron spin states with respect to the external magnetic field. This subsequently leads to no phase contrast signal but a loss of interferometer visibility referred to as dark-field contrast. We demonstrate how the implementation of spin analysis to the Talbot-Lau interferometer setup enables one to recover the differential phase induced to a single spin state. Thus, we show that the dark-field contrast is a measure of the quantum mechanical spin split analogous to the Stern-Gerlach experiment without, however, spatial beam separation. In addition, the spin analyzed dark-field contrast imaging introduced here bears the potential to probe polarization dependent small-angle scattering and thus magnetic microstructures.

5.
ACS Appl Mater Interfaces ; 12(25): 28461-28473, 2020 Jun 24.
Article in English | MEDLINE | ID: mdl-32330001

ABSTRACT

The initial formation stages of surfactant-templated silica thin films which grow at the air-water interface were studied using combined spin-echo modulated small-angle neutron scattering (SEMSANS) and small-angle neutron scattering (SANS). The films are formed from either a cationic surfactant or nonionic surfactant (C16EO8) in a dilute acidic solution by the addition of tetramethoxysilane. Previous work has suggested a two stage formation mechanism with mesostructured particle formation in the bulk solution driving film formation at the solution surface. From the SEMSANS data, it is possible to pinpoint accurately the time associated with the formation of large particles in solution that go on to form the film and to show their emergence is concomitant with the appearance of Bragg peaks in the SANS pattern, associated with the two-dimensional hexagonal order. The combination of SANS and SEMSANS allows a complete depiction of the steps of the synthesis that occur in the subphase.

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