XAFCA: a new XAFS beamline for catalysis research

Du, Yonghua; Zhu, Yi; Xi, Shibo; Yang, Ping; Moser, H. O.; Breese, Mark B. H.; Borgna, Armando

doi:10.1107/s1600577515002854

Cited by 140 publications

(105 citation statements)

References 6 publications

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“…During the structural transformation the formation of a Cd 2 O 2 ring is expected. Such a dinuclear core can template the axially coordinated 4‐spy ligands to come closer with the parallel orientation and satisfy the Schmidt’s topochemical criteria (<4.2 Å) 7. Thus a completely desolvated 1 , that is, the proposed 2D CP structure, is expected to be photoreactive.…”

Section: Methodsmentioning

confidence: 98%

“…XAFS measurements : XAFS experiments were carried out at the XAFCA beamline,7 Singapore Synchrotron Light Source (SSLS). The electron storage ring of SSLS is operated with an energy of 0.7 GeV with 200–300 mA current.…”

Section: Methodsmentioning

confidence: 99%

“…Crystal data for1: T = 100(2) K, C 40 H 46 CdN 4 O 9 , Mr = 839.21, monoclinic, C2/c; a = 30.851(9), b = 6.0083(14), c = 21.833(5) , b = 111.173(4)8, V = 3773.9(16) 3 , Z = 4, 1 calcd = 1.477 gcm À3 , m = 0.640 mm À1 ,G OF = 1.091, final R1 = 0.0380, wR2 = 0.0952 [for 3987 data I > 2s(I)].C CDC 938967 contains the supplementary crystallographic data. These data can be obtained free of charge by The Cambridge Crystallographic Data Centre XAFS measurements:X AFS experiments were carried out at the XAFCA beamline, [7] Singapore Synchrotron Light Source (SSLS). The electron storage ring of SSLS is operated with an energy of 0.7 GeV with 200-300 mA current.…”

Section: Methodsmentioning

confidence: 99%

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A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

Medishetty

Tandiana

et al. 2015

Chemistry A European J

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Two solid-state structural transformations that occur in a stepwise and a controlled manner are described. A combination of desolvation and cycloaddition reactions has been employed to synthesise a 3D coordination polymer (CP) from 1D CP [Cd(bdc)(4-spy)2 (H2 O)]⋅2 H2 O⋅2 DMF (bdc=1,4-benzenedicarboxylate, 4-spy=4-styrylpyridine) presumably via a 2D layered structure, [Cd2 (bdc)2 (4-spy)4 ]. In the absence of single crystals to follow the course of the photocycloaddition reaction, thermogravimetry, XAFS and NOESY NMR experiments were used to propose the formation of layered and pillared layered structures. Further, the present strategy enables us to synthesise new multidimensional architectures that are otherwise inaccessible by the self-assembly process.

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Section: Methodsmentioning

confidence: 98%

Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

Medishetty

Tandiana

et al. 2015

Chemistry A European J

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“…[51] A custom-designed cell was employed to carry out the operando measurement under transmission mode. [51] A custom-designed cell was employed to carry out the operando measurement under transmission mode.…”

Section: Methodsmentioning

confidence: 99%

Na₃V₂(PO₄)₃ as the Sole Solid Energy Storage Material for Redox Flow Sodium‐Ion Battery

Zhou

Chen

Zhang

et al. 2019

Advanced Energy Materials

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like wind and solar for electricity generation. The growth will go on accelerating to replace the fossil fuels in the future. [1] At the same time, the intermittent nature of these power sources necessitates a durable and cost-effective energy storage system to meet the huge demands for peak shifting and power buffering for GWscale systems. Considering the scalability, operation safety, and flexibility, redox flow battery (RFB) is regarded as one of the most promising electrochemical energy storage technologies which have found their own niche for the large-scale energy storage applications. [2] Unlike other rivals such as lithium ion battery and leadacid battery, RFB stores energy in mobilized electrolyte solutions other than in solid active materials coated on electrode sheets. The design that the redox active compounds circulate between the storage reservoir and cell stack with the aid of pumps, enables decoupled energy storage and power generation.However, the conventional redox flow batteries severely suffer from low energy density (<40 Wh L −1 ) as a result of limited solubility of redox species and low cell voltage, which adds on the footprint and capital cost of the system, impeding its practical deployment. [3] To improve the energy density, various aprotic RFBs have been explored for enhanced cell voltage. [4,5] However, because of the low solubility of aprotic solvents to many redox active compounds, [6] the reported high energy aprotic RFBs are limited to a few systems such as polyiodide, [7] redox-active ionic liquids, [8,9] deep eutectics, [10] and hybrid electrolyte. [11,12] Through molecular engineering, metallocene such as ferrocene derivatives [13,14] and redox-active organic materials [15][16][17][18][19] such as 2,2,6,6-tetramethylpiperidin-1-oxyl derivatives [17] and benzothiadiazole [16] have recently been reported to have good solubility and potentially high energy density. Although the solubility can reach up to 5 m in pure solvent, taking the supporting salts and electrolyte viscosity into consideration, the practical concentration of those molecules remains limited to <2 m.[2] By forming slurry of solid active materials with conducting carbon additives, semisolid flow cells that utilize solid suspensions represent an alternative way to increase the effective concentration. [20] Although the energy density can in theory be increased considerably, these cells may have critical issues on fluid conductivities and Redox flow batteries have considerable advantages of system scalability and operation flexibility over other battery technologies, which makes them promising for large-scale energy storage application. However, they suffer from low energy density and consequently relatively high cost for a nominal energy output. Redox targeting-based flow batteries are employed by incorporating solid energy storage materials in the tank and present energy density far beyond the solubility limit of the electrolytes. The success of this concept relies on paring suitable redox mediators with solid mate...

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“…X-ray absorption spectra (XAS) of Ni K-edge and W L 3 -edge were recorded at the XAFCA beamline at the Singapore Synchrotron Light Source. [45] The samples were first mixed and ground thoroughly with boron nitride, followed by pressing the sample into a small wafer with a diameter of 1 cm. The catalysts were reduced with H 2 inside the chamber at 500 8C for 2 h, purged with flowing He and then cooled down to room temperature.…”

Section: Catalyst Characterizationmentioning

confidence: 99%

C−O Hydrogenolysis of Tetrahydrofurfuryl Alcohol to 1,5‐Pentanediol Over Bi‐functional Nickel‐Tungsten Catalysts

Soghrati

Poh

et al. 2018

ChemCatChem

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In this study, we report a series of bimetallic Ni−WOx catalyst for the ring‐opening of THFA into 15PDO. The structure‐performance relationship of the catalysts was discussed based on extensive characterization using techniques such as BET, H2‐TPR, NH3‐TPD, Pyr‐IR, IPA‐TPD‐MS, XRD, XPS and EXAFS/XANES. The acidity measurements show that higher W density leads to the higher amount of acid density, which could be assigned to the creation of Lewis acid sites mainly on the surface of the calcined catalysts. H2‐TPR profiles of Ni−WOx catalysts show that there is a strong interaction between Ni and W species, enhancing the reducibility of WOx. XRD measurements of calcined Ni−WOx catalysts reveal that the dispersion of Ni particles is enhanced after addition of WOx species. After reduction, different peaks corresponding to metallic Ni and WO3−x are identified for 10Ni−WOx catalysts, as well as new peak assigned to Ni−W intermetallic phase on 10Ni−30WOx catalyst. The formation of Ni−W intermetallic phase was further proved using XPS and EXAFS studies. THFA hydrogenolysis was also conducted under aqueous‐phase conditions over Ni−WOx catalysts, yielding up to 47 % selectivity to 15PDO, along with a highest combined C5 polyols (i. e., 15PDO and 125PTO) selectivity of approximately 64 %. However, the Ni−WOx catalytic system suffers from deactivation process due to the hydrothermal dissolution of the active phase. Further investigation reveals the better stability of metallic tungsten and Ni−W intermetallic phase (Ni4W) against leaching since their corresponding peaks in the XRD patterns of spent catalysts remains nearly unchanged. Finally, 1,4‐dioxane as an organic solvent was employed in THFA hydrogenolysis reaction, resulting in different product distribution, with a THP yield of around 54 %. The catalyst crystalline structure is preserved because of very low Ni and W leaching when 1,4‐dioxane is used as solvent.

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XAFCA: a new XAFS beamline for catalysis research

Cited by 140 publications

References 6 publications

A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

Na₃V₂(PO₄)₃ as the Sole Solid Energy Storage Material for Redox Flow Sodium‐Ion Battery

C−O Hydrogenolysis of Tetrahydrofurfuryl Alcohol to 1,5‐Pentanediol Over Bi‐functional Nickel‐Tungsten Catalysts

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XAFCA: a new XAFS beamline for catalysis research

Cited by 140 publications

References 6 publications

A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

A Step‐by‐Step Assembly of a 3D Coordination Polymer in the Solid‐State by Desolvation and [2+2] Cycloaddition Reactions

Na3V2(PO4)3 as the Sole Solid Energy Storage Material for Redox Flow Sodium‐Ion Battery

C−O Hydrogenolysis of Tetrahydrofurfuryl Alcohol to 1,5‐Pentanediol Over Bi‐functional Nickel‐Tungsten Catalysts

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Na₃V₂(PO₄)₃ as the Sole Solid Energy Storage Material for Redox Flow Sodium‐Ion Battery