(Invited) In Situ Synchrotron x-Ray Spectroscopic Studies of Energy Materials

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.


2018 ◽  
Vol 941 ◽  
pp. 943-948
Author(s):  
Katja Hauschildt ◽  
Andreas Stark ◽  
Hilmar Burmester ◽  
Ursula Tietze ◽  
Norbert Schell ◽  
...  

TiAl alloys are increasingly used as a lightweight material, for example in aero engines, which also leads to the requirement for suitable repair techniques. Transient liquid phase bonding is a promising method for the closure of cracks (in non-critical or non-highly loaded areas). The brazing solder Ti-24Ni was investigated for brazing the alloy Ti-45Al-5Nb-0.2B-0.2C (in at. %). After brazing, the joint exhibits different microstructures and phase compositions. The transient liquid phase bonding process was investigated in the middle of the joint region in situ to acquire time resolved information of the phases, their development, and thus the brazing process. These investigations were performed using high-energy X-ray diffraction at the “High-Energy Materials Science” beamline HEMS, located at the synchrotron radiation facility PETRA III at DESY in Hamburg, Germany. For this, we used an induction furnace, which is briefly described here. During the analysis of the diffraction data with Rietveld refinement, the amount of liquid was refined with Gaussian peaks and thus could be quantified. Furthermore, while brazing four different phases occurred in the middle of the joint region over time. Additionally, the degree of ordering of the βo phase was determined with two ideal stoichiometric phases (completely ordered and disordered). Altogether, the phase composition changed clearly over the first six hours of the brazing process.


2021 ◽  
Vol 28 (6) ◽  
Author(s):  
T.-L. Hsiung ◽  
L.-W. Wei ◽  
H.-L. Huang ◽  
H. Paul Wang

Toxic disinfection byproducts such as trihalomethanes (e.g. CHCl3) are often found after chlorination of drinking water. It has been found that photocatalytic degradation of trace CHCl3 in drinking water generally lacks an expected relationship with the crystalline phase, band-gap energy or the particle sizes of the TiO2-based photocatalysts used such as nano TiO2 on SBA-15 (Santa Barbara amorphous-15), TiO2 clusters (TiO2–SiO2) and atomic dispersed Ti [Ti-MCM-41 (Mobil Composition of Matter)]. To engineer capable TiO2 photocatalysts, a better understanding of their photoactive sites is of great importance and interest. Using in situ X-ray absorption near-edge structure (XANES) spectroscopy, the A1 (4969 eV), A2 (4971 eV) and A3 (4972 eV) sites in TiO2 can be distinguished as four-, five- and six- coordinated Ti species, respectively. Notably, the A2 Ti sites that are the main photocatalytic species of TiO2 are shown to be accountable for about 95% of the photocatalytic degradation of trace CHCl3 in drinking water (7.2 p.p.m. CHCl3 gTiO2 −1 h−1). This work reveals that the A2 Ti species of a TiO2-based photocatalyst are mainly responsible for the photocatalytic reactivity, especially in photocatalytic degradation of CHCl3 in drinking water.


1990 ◽  
Vol 137 (2) ◽  
pp. 383-388 ◽  
Author(s):  
K. I. Pandya ◽  
R. W. Hoffman ◽  
J. McBreen ◽  
W. E. O'Grady

2015 ◽  
Vol 200 ◽  
pp. 264-273 ◽  
Author(s):  
Ethan J. Crumlin ◽  
Zhi Liu ◽  
Hendrik Bluhm ◽  
Wanli Yang ◽  
Jinghua Guo ◽  
...  
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