Commissioning and first results of scanning type EXAFS beamline (BL-09) at INDUS-2 synchrotron source

Poswal, A.K.; Agrawal, Ankur; Yadav, Ashok K.; Nayak, Chandrani; Basu, Shibom; Kane, S. R.; Garg, C. K.; Bhattachryya, D.; Jha, S. N.; Sahoo, N. K.

doi:10.1063/1.4872706

Cited by 128 publications

(59 citation statements)

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“…An XAS measurement comprising of both XANES and EXAFS was studied at Cu K‐edge to probe the local structure of the samples. XAS was recorded using energy‐scanning EXAFS beamline (BL‐9), Indus‐2 Synchrotron Source (2.5 GeV, 100 mA), at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore, India …”

Section: Methodsmentioning

confidence: 99%

“…XAS was recorded using energyscanning EXAFS beamline (BL-9), Indus-2 Synchrotron Source (2.5 GeV, 100 mA), at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore, India. 30,31 2.3 | Hydrolysis CuCl 2 hydrolysis was performed in a fixed bed quartz reactor (length 50 cm, OD 1.2 cm, Figure 1), in which approximately 0.3-g reactant (UBM, BM3, BM6 and BM12) was immobilized using quartz wool. During experiments, the flow of water was regulated by syringe pump.…”

Section: Characterizationmentioning

confidence: 99%

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Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

et al. 2019

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Summary Detailed investigations of CuCl2 hydrolysis step of Cu–Cl thermochemical cycle were carried out on various aspects: (a) characterization and thermal properties of reactants/products using X‐ray diffraction (XRD), thermogravimetry–mass spectrometry (TG‐MS), scanning electron microscopy (SEM), temperature‐programmed desorption (TPD), and extended X‐ray absorption fine structure (EXAFS); (b) performance evaluation of fixed bed hydrolysis; (c) parametric optimization with respect to S/Cu, flow rate (gas hourly space velocity, GHSV), reaction duration, temperature, and particle size; and (d) monitored hydrolysis using isothermal TG experiments at 360°C, 370°C, 380°C, 390°C, and 400°C to derive kinetic parameters rate constant (k) and activation energy (Ea) on the basis of the shrinking‐core model. 97% conversion to Cu2OCl2 at 17 630 h−1 of GHSV, 400°C was achieved using ball‐milled CuCl2 (BM6), as compared with that of 55% over commercial un–ball‐milled reactant, CuCl2 (UBM). Correspondingly, higher k value of 2.84 h−1 over BM6 as compared with 0.97 h−1 over UBM reactant at 400°C was achieved. Ea for hydrolysis of BM6 was 93 kJ/mol, while it was 106 kJ/mol for UBM as derived from the Arrhenius plot. A probable pathway for CuCl2 hydrolysis is proposed here. It was found to be diffusion controlled, and the particle size of reactant molecules affects the packing and diffusion length. Based on our investigations, it is very unlikely to get >99% phase pure product (Cu2OCl2). Cu2OCl2 is labile in nature and tends to transform into structurally similar and stable compounds CuO and CuCl2.

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Section: Methodsmentioning

confidence: 99%

Section: Characterizationmentioning

confidence: 99%

Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

et al. 2019

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“…41,42 Photon energy range of the beamline is 4-25 keV. Beamline optics consists of a Rh/Pt coated collimating meridional cylindrical mirror used for collimation of beam.…”

Section: Methodsmentioning

confidence: 99%

Effect of ionic size compensation by Ag⁺ incorporation in homogeneous Fe-substituted ZnO: studies on structural, mechanical, optical, and magnetic properties

et al. 2018

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Substituting an ion of different size from that of the host element introduces lattice strain and defects.However, this mismatch may be significantly reduced by substituting an additional ion with a compensating size relative to the dopant. Such a double substitution might offer better solubility irrespective of the local distortions as well as the formation of defects in the valence states. Fesubstituted ZnO has been widely reported with conflicting results primarily arising from lack of chemical and structural homogeneity originating from preparation techniques, compositional fluctuations, and equivocal comprehension of actual solubility limits of the dopants. In this study, Ag ion has been incorporated in Fe-substituted ZnO to compensate the ionic size of Zn 1Àx [Fe 0.8

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“…X‐ray absorption spectroscopy measurements were carried out for the films in both the transmission and fluorescence modes as required. Energy‐scanning EXAFS beam‐line (BL‐9) at the Indus‐2 Synchrotron Source (2.5 GeV, 100 mA) installed at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore, India was utilized to carry out EXAFS and XANES measurements on the films deposited here. Operating energy range was 4 to 25 keV.…”

Section: Resultsmentioning

confidence: 99%

Probing local structures in (Ni/Co)‐codoped ZnO/PVDF composite flexible and freestanding films by using XAS and XPS studies

et al. 2018

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Extended X‐ray absorption fine‐structure and X‐ray absorption near‐edge structure studies have been performed on five Ni/Co‐codoped ZnO/polyvinylidene fluoride composite flexible and freestanding films to probe the local structure surrounding the Zn, Co, and Ni sites. X‐ray photoelectron spectroscopy studies are also performed for throwing insight in charge states of Co and Ni being incorporated. X‐ray absorption near‐edge structure studies confirmed the incorporation of Co atoms at tetrahedral sites of the wurtzite host matrix. They acted as substitutional impurities without forming any detectable impurity phase or cobalt clusters.

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Commissioning and first results of scanning type EXAFS beamline (BL-09) at INDUS-2 synchrotron source

Cited by 128 publications

References 1 publication

Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

Effect of ionic size compensation by Ag⁺ incorporation in homogeneous Fe-substituted ZnO: studies on structural, mechanical, optical, and magnetic properties

Probing local structures in (Ni/Co)‐codoped ZnO/PVDF composite flexible and freestanding films by using XAS and XPS studies

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Commissioning and first results of scanning type EXAFS beamline (BL-09) at INDUS-2 synchrotron source

Cited by 128 publications

References 1 publication

Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

Investigations on the hydrolysis step of copper‐chlorine thermochemical cycle for hydrogen production

Effect of ionic size compensation by Ag+ incorporation in homogeneous Fe-substituted ZnO: studies on structural, mechanical, optical, and magnetic properties

Probing local structures in (Ni/Co)‐codoped ZnO/PVDF composite flexible and freestanding films by using XAS and XPS studies

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Effect of ionic size compensation by Ag⁺ incorporation in homogeneous Fe-substituted ZnO: studies on structural, mechanical, optical, and magnetic properties