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Instruments / Technical Area	Publication Details	Published
I05-ARPES	Cubic rashba effect in the surface spin structure of rare-earth ternary materials D. y. Usachov , I. a. Nechaev , G. Poelchen , M. Guttler , E. e. Krasovskii , S. Schulz , A. Generalov , K. Kliemt , A. Kraiker , C. Krellner , K. Kummer , S. Danzenbächer , C. Laubschat , A. p. Weber , J. Sánchez-Barriga , E. v. Chulkov , A. f. Santander-Syro , T. Imai , K. Miyamoto , T. Okuda , D. V. Vyalikh Physical Review Letters 124 DOI: 10.1103/PhysRevLett.124.237202 Diamond Proposal Number(s): [18844, 17761] Show Abstract ▼ Abstract: Spin-orbit interaction and structure inversion asymmetry in combination with magnetic ordering is a promising route to novel materials with highly mobile spin-polarized carriers at the surface. Spin-resolved measurements of the photoemission current from the Si-terminated surface of the antiferromagnet TbRh 2 Si 2 and their analysis within an ab initio one-step theory unveil an unusual triple winding of the electron spin along the fourfold-symmetric constant energy contours of the surface states. A two-band k ⋅ p model is presented that yields the triple winding as a cubic Rashba effect. The curious in-plane spin-momentum locking is remarkably robust and remains intact across a paramagnetic-antiferromagnetic transition in spite of spin-orbit interaction on Rh atoms being considerably weaker than the out-of-plane exchange field due to the Tb 4 f moments.	Jun 2020
	The significance of bromide in the Brust–Schiffrin synthesis of thiol protected gold nanoparticles S. G. Booth , A. Uehara , Sin-Yuen Chang , C. La Fontaine , T. Fujii , Y. Okamoto , T. Imai , S. L. M. Schroeder , R. A. W. Dryfe Chemical Science 8, 7954 - 7962 DOI: 10.1039/C7SC03266H Open Access Show Abstract ▼ Abstract: The mechanism of the two-phase Brust–Schiffrin synthesis of alkane thiol protected metal nanoparticles is known to be highly sensitive to the precursor species and reactant conditions. In this work X-ray absorption spectroscopy is used in conjunction with liquid/liquid electrochemistry to highlight the significance of Br− in the reaction mechanism. The species [AuBr4]− is shown to be a preferable precursor in the Brust–Schiffrin method as it is more resistant to the formation of Au(I) thiolate species than [AuCl4]−. Previous literature has demonstrated that avoidance of the Au(I) thiolate is critical to achieving a good yield of nanoparticles, as [Au(I)X2]− species are more readily reduced by NaBH4. We propose that the observed behavior of [AuBr4]− species described herein explains the discrepancies in reported behavior present in the literature to date. This new mechanistic understanding should enable nanoparticle synthesis with a higher yield and reduce particle size polydispersity.	Sep 2017
B18-Core EXAFS I18-Microfocus Spectroscopy	Electrochemical insight into the brust–schiffrin synthesis of Au nanoparticles Akihiro Uehara , Samuel Booth , Sin-Yuen Chang , Sven L. M. Schroeder , Takahito Imai , Teruo Hashimoto , J. Frederick W. Mosselmans , Robert A. W. Dryfe Journal Of The American Chemical Society 137 (48), 15135–15144 DOI: 10.1021/jacs.5b07825 PMID: 26559785 Diamond Proposal Number(s): [11293, 8861] Open Access Show Abstract ▼ Abstract: The mechanism of the Brust-Schiffrin gold nanoparticle synthesis has been investigated through the use of ion transfer voltammetry at the water\|1,2-dichloroethane (DCE) solution interface, combined with X-ray absorption fine structure (XAFS) of the reaction between [AuCl4]- and thiol (RSH) in homogeneous toluene (TL) solution. Ion transfer calculations indi- cate the formation of [AuCl2]- at RSH:Au ratios from 0.2 – 2 with a time-dependent variation observed over several days. At RSH:Au ratios above 2 and after time periods greater than 24 hours, the formation of Au(I)SR is also observed. The relative concentrations of reaction products observed at the liquid/liquid interface are in excellent agreement with those observed by XAFS for the corresponding reaction in a single homogeneous phase. BH4- ion transfer reactions between water and DCE indicate that the reduction of [AuCl4]- and/or [AuCl2]- to Au nanoparticles by BH4- proceeds in the bulk organic phase. On the other hand, BH4- was unable to reduce the insoluble [Au(I)SR]n species to Au nanoparticles. The number and size of the nanoparticles formed was dependent on the concentration ratio of RSH:Au, as well as the experimental duration because of the competing formation of the [Au(I)SR]n precipitate. Higher concentrations of nanoparticles, with diameters of 1.0 – 1.5 nm, were formed at RSH:Au ratios from 1 to 2.	Nov 2015

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