In Situ X-Ray Absorption Spectroscopy Studies of Functional Nanomaterials

  • Soma Chattopadhyay
  • Soon Gu Kwon
  • Elena V. Shevchenko
  • Jeffrey T. Miller
  • Steve M. Heald


X-ray absorption spectroscopy (XAS) is a powerful technique to study the unoccupied states and the local structure around an excited species of atoms from an element present in a material. Recently, in situ XAS is being used to study catalytic transformations, synthesis of nanoparticles and thin films, kinetics of potential battery materials, etc. Such studies can explain the mechanisms associated with the formation of chemical species during various types of reactions. In this chapter, we shall describe how XAS has proved to be a powerful characterization tool for nanomaterials with potential applications by determining the variation in interatomic distances, coordination numbers, and the type of neighboring atoms within the first few coordination shells of the atom of interest in nanoparticles.


  1. 1.
    Koningsberger DC, Prins R (1988) X-ray absorption, principles, applications, techniques of EXAFS, SEXAFS, XANES. Wiley, New YorkGoogle Scholar
  2. 2.
    Müller O, Nachtegaal M, Just J, Lützenkirchen-Hecht D, Frahm R (2016) Quick-EXAFS setup at the SuperXAS beamline for in situ X-ray absorption spectroscopy with 10 ms time resolution. J Synchrotron Radiat 23(1):260–266Google Scholar
  3. 3.
    Prestipino C, Mathon O, Hino R, Beteva A, Pascarelli S (2011) Quick-EXAFS implementation on the general purpose EXAFS beamline at ESRF. J Synchrotron Radiat 18(2):176–182Google Scholar
  4. 4.
    Mathon O, Beteva A, Borrel J, Bugnazet D, Gatla S, Hino R, Kantor I, Mairs T, Munoz M, Pasternak S, Perrin F, Pascarelli S (2015) The time-resolved and extreme condition XAS (TEXAS) facility at the European Synchrotron Radiation Facility: the general-purpose EXAFS bending-magnet beamline BM23. J Synchrotron Radiat 22(6):1548–1554Google Scholar
  5. 5.
    Koide A, Fujikawa T, Ichikuni N (2014) Recent progress in EXAFS/NEXAFS spectroscopy. J Electron Spectrosc Relat Phenom 195:375–381Google Scholar
  6. 6.
    Dent AJ (2002) Development of time-resolved XAFS instrumentation for quick EXAFS and energy-dispersive EXAFS measurements of catalyst systems. Top Catal 18(1–2):14–22Google Scholar
  7. 7.
    Segre CU, Leyarovska NE, Chapman LD, Lavender WM, Plag PW, King AS, Kropf AJ, Bunker BA, Kemner KM, Dutta P, Duran RS, Kaduk J (2000) The MRCAT insertion device beamline at the advanced photon source. AIP Conf Proc 521(1):419–422Google Scholar
  8. 8.
    Newville M (2004) Fundamentals of XAFS. Consortium for advanced radiation sources, University of Chicago, Chicago. Scholar
  9. 9.
    Lee PA, Citrin PH, Eisenberger P, Kincaid BM (1981) Extended X-ray absorption fine structure – its strengths and limitations as a structural tool. Rev Mod Phys 53(4):769Google Scholar
  10. 10.
    Rehr JJ, Albers RC (2000) Theoretical approaches to X-ray absorption fine structure. Rev Mod Phys 72(3):621Google Scholar
  11. 11.
    Bunker G (2010) Introduction to XAFS: a practical guide to X-ray absorption fine structure spectroscopy, 1st edn. Cambridge University Press, CambridgeGoogle Scholar
  12. 12.
    Kelly SD, Hesterberg D, Ravel B (2008) Chapter 14 Analysis of soils and minerals using X-ray absorption spectroscopy. In: Methods of soil analysis Part 5 – Mineralogical methods. Soil Science Society of America, Madison, pp 387–463Google Scholar
  13. 13.
    Ravel B, Newville M (2005) ATHENA, ARTEMIS, HEPHAESTUS: data analysis for X-ray absorption spectroscopy using IFEFFIT. J Synchrotron Radiat 12(4):537–541Google Scholar
  14. 14.
    Zabinsky SI, Rehr JJ, Andukinov A, Albers RC, Ellen MJ (1995) Multiple-scattering calculations of X-ray absorption spectra. Phys Rev B 52(4):2995Google Scholar
  15. 15.
    Kumar CSSR (ed) (2010) Microfluidic devices in nanotechnology – fundamental concepts. Wiley, HobokenGoogle Scholar
  16. 16.
    Kumar CSSR (ed) (2010) Microfluidic devices in nanotechnology – applications. Wiley, HobokenGoogle Scholar
  17. 17.
    Gaur S, Miller JT, Stellwagen DR, Sanampudi A, Kumar CSSR, Spivey JJ (2012) Synthesis, characterization and testing of supported Au catalysts prepared from atomically-tailored Au38(SC12H25)24 clusters. Phys Chem Chem Phys 14(5):1627–1634Google Scholar
  18. 18.
    Biswas S, Miller JT, Li Y, Nandakumar K, Kumar CSSR (2012) Developing a millifluidic platform for the synthesis of ultra-small nano-clusters: ultra-small copper nano-clusters as a case study. Small 8(5):688–698Google Scholar
  19. 19.
    Krishna KS, Navin CV, Biswas S, Singh V, Ham K, Bovenkamp GL, Theegala CS, Miller JT, Spivey J, Kumar CSSR (2013) Milli-fluidics for time-resolved mapping of the growth of gold nanostructures. J Am Chem Soc 135(14):5450–5456Google Scholar
  20. 20.
    Krishna KS, Biswas S, Navin CV, Yamane DG, Miller JT, Kumar CSSR (2013) Millifluidics for chemical synthesis and time-resolved mechanistic studies. J Vis Exp 81:e50711Google Scholar
  21. 21.
    Navin CV, Krishna KS, Bovenkamp GL, Miller JT, Chattopadhyay S, Shibata T, Losovyj Y, Singh V, Theegala C, Kumar CSSR (2015) Investigation of the synthesis and characterization of platinum-DMSA nanoparticles using millifluidic chip reactor. Chem Eng J 281:81–86Google Scholar
  22. 22.
    Yin Y, Alivisatos AP (2005) Colloidal nanocrystal synthesis and the organic–inorganic interface. Nature 437(7059):664–670Google Scholar
  23. 23.
    Pellegrino T, Kudera S, Liedl T, Javier AM, Manna L, Parak WJ (2005) On the development of colloidal nanoparticles towards multifunctional structures and their possible use for biological applications. Small 1(1):48–63Google Scholar
  24. 24.
    Talapin DV, Lee J-S, Kovalenko MV, Shevchenko EV (2010) Prospects of colloidal nanocrystals for electronic and optoelectronic applications. Chem Rev 110(1):389–458Google Scholar
  25. 25.
    Park J, Joo J, Kwon SG, Jang Y, Hyeon T (2007) Synthesis of monodisperse spherical nanocrystals. Angew Chem Int Ed 46(25):4630–4660Google Scholar
  26. 26.
    Kwon SG, Krylova G, Phillips PJ, Klie RF, Chattopadhyay S, Shibata T, Bunel EE, Liu Y, Prakapenka VB, Lee B, Shevchenko EV (2015) Heterogeneous nucleation and shape transformation of multicomponent metallic nanostructures. Nat Mater 14(2):215–223Google Scholar
  27. 27.
    Kwon SG, Chattopadhyay S, Koo B, dos Santos Claro PC, Shibata T, Requejo FG, Giovanetti LJ, Johnson C, Prakapenka V, Lee B, Shevchenko EV (2016) Oxidation induced doping of nanoparticles revealed by in situ X-ray adsorption studies. Nano Lett 16(6):3738–3747Google Scholar
  28. 28.
    McPeak KM, Becker MA, Britton NG, Majidi H, Bunker BA, Baxter JB (2010) In situ X-ray absorption near-edge structure spectroscopy of ZnO nanowire growth during chemical bath deposition. Chem Mater 22(22):6162–6170Google Scholar
  29. 29.
    Song J, Zhang J, Xie Z, Wei S, Pan Z, Hu T, Xie Y (2010) In situ XAFS studies on the growth of ZnSe quantum dots. Nucl Instrum Methods Phys Res, Sect A 619(1–3):280–282Google Scholar
  30. 30.
    Yan H, Mayanovic RA, Demster JW, Anderson AJ (2013) In situ monitoring of the adsorption of Co2+ on the surface of Fe3O4 nanoparticles in high-temperature aqueous fluids. J Supercrit Fluids 81:175–182Google Scholar
  31. 31.
    Tryk DA, Bae IT, Hu Y, Kim S, Antonio MR, Schersona DA (1995) In situ X-ray absorption fine structure measurements of LaNi5 electrodes in alkaline electrolytes. J Electrochem Soc 142(3):824–828Google Scholar
  32. 32.
    Shiraishi Y, Nakai I, Tsubata T, Himeda T, Nishikawa F (1997) In situ transmission X-ray absorption fine structure analysis of the charge–discharge process in LiMn2O4, a rechargeable lithium battery material. J Solid State Chem 133(2):587–590Google Scholar
  33. 33.
    Balasubramanian M, Sun X, Yang XQ, McBreen J (2001) In situ X-ray diffraction and X-ray absorption studies of high-rate lithium-ion batteries. J Power Sources 92(1–2):1–8Google Scholar
  34. 34.
    Terada Y, Yasaka K, Nishikawa F, Konishi T, Yoshio M, Nakai I (2001) In situ XAFS analysis of Li(Mn,M)2O4 (M = Cr, Co, Ni) 5V cathode materials for lithium-ion secondary batteries. J Solid State Chem 156(2):286–291Google Scholar
  35. 35.
    Kropf AJ, Tostmann H, Johnson CS, Vaughey JT, Thackeray MM (2001) An in situ X-ray absorption spectroscopy study of InSb electrodes in lithium batteries. Electrochem Commun 3(5):244–251Google Scholar
  36. 36.
    Balasubramanian M, McBreen J, Davidson IJ, Whitfield PS, Kargina I (2002) In situ X-ray absorption study of a layered manganese-chromium oxide-based cathode material. J Electrochem Soc 149(2):A176–A184Google Scholar
  37. 37.
    Johnson CS, Kropf AJ (2002) In situ XAFS analysis of the LixNi0.8Co0.2O2 cathode during cycling in lithium batteries. Electrochim Acta 47(19):3187Google Scholar
  38. 38.
    Holzapfel M, Proux O, Strobel P, Darie C, Borowski M, Morcrette M (2004) Effect of iron on delithiation in LixCo1−yFeyO2: part 2, in-situ XANES and EXAFS upon electrochemical cycling. J Mater Chem 14(1):102–110Google Scholar
  39. 39.
    Yoon W-S, Balasubramanian M, Chung KY, Yang X-Q, McBreen J, Grey CP, Fischer DA (2005) Investigation of the charge compensation mechanism on the electrochemically Li-ion deintercalated Li1-xCo1/3Ni1/3Mn1/3O2 electrode system by combination of soft and hard X-ray absorption spectroscopy. J Am Chem Soc 127(49):17479–17487Google Scholar
  40. 40.
    Deb A, Bergmann U, Cramer SP, Cairns EJ (2005) In-situ X-ray absorption spectroscopic study of the Li [Ni1/3Co1/3Mn1/3]O2 cathode material. J Appl Phys 97(11):113523Google Scholar
  41. 41.
    Deb A, Cairns EJ (2006) In situ X-ray absorption spectroscopy – a probe of cathode materials for Li-ion cells. Fluid Phase Equilib 241(1–2):4–19Google Scholar
  42. 42.
    Dominko R, Arčon I, Kodre A, Hanžel D, Gaberšček M (2009) In-situ XAS study on Li2MnSiO4 and Li2FeSiO4 cathode materials. J Power Sources 189(1):51–58Google Scholar
  43. 43.
    Nedoseykina T, Kim MG, Park S-A, Kim H-S, Kim S-B, Cho J, Lee Y (2010) In situ X-ray absorption spectroscopic study for the electrochemical delithiation of a cathode LiFe0.4Mn0.6PO4 material. Electrochim Acta 55(28):8876–8882Google Scholar
  44. 44.
    Ito A, Sato Y, Sanada T, Hatano M, Horie H, Ohsawa Y (2011) In situ X-ray absorption spectroscopic study of Li-rich layered cathode material Li[Ni0.17Li0.2Co0.07Mn0.56]O2. J Power Sources 196(16):6828–6834Google Scholar
  45. 45.
    Simonin L, Colin J-F, Ranieri V, Canévet E, Martin J-F, Bourbon C, Baehtz C, Strobel P, Daniel L, Patoux S (2012) In-situ investigations of a Li-rich Mn-Ni layered oxide for Li-ion batteries. J Mater Chem 22(22):11316–11322Google Scholar
  46. 46.
    Love CT, Korovina A, Patridge CJ, Swider-Lyons KE, Twigg ME, Ramaker DE (2013) Review of LiFePO4 phase transition mechanisms and new observations from X-ray absorption spectroscopy. J Electrochem Soc 160(5):A3153–A3161Google Scholar
  47. 47.
    Pohl AH, Guda AA, Shapovalov VV, Witte R, Das B, Scheiba F, Rothe J, Soldatov AV, Fichtner M (2014) Oxidation state and local structure of a high-capacity LiF/Fe(V2O5) conversion cathode for Li-ion batteries. Acta Mater 68:179–188Google Scholar
  48. 48.
    Hirsch O, Zeng G, Luo L, Staniuk M, Abdala PM, van Beek W, Rechberger F, Süess MJ, Niederberger M, Koziej D (2014) Aliovalent Ni in MoO lattice – probing the structure and valence of Ni and its implication on the electrochemical performance. Chem Mater 26(15):4505–4513Google Scholar
  49. 49.
    Pelliccione CJ, Ding Y, Timofeeva EV, Segre CU (2015) In situ XAFS study of the capacity fading mechanisms in ZnO anodes for lithium-ion batteries. J Electrochem Soc 162(10):A1935–A1939Google Scholar
  50. 50.
    Li B, Shao R, Yan H, An L, Zhang B, Wei H, Ma J, Xia D, Han X (2016) Understanding the stability for Li-rich layered oxide Li2RuO3 cathode. Adv Funct Mater 26(9):1330–1337Google Scholar
  51. 51.
    Mansour AN, Badway F, Yoon WS, Chung KY, Amatucci GG (2010) In situ X-ray absorption spectroscopic investigation of the electrochemical conversion reactions of CuF2-MoO3 nanocomposite. J Solid State Chem 183(12):3029–3038Google Scholar
  52. 52.
    Pelliccione CJ, Timofeeva EV, Segre CU (2016) Potential-resolved in situ X-ray absorption spectroscopy study of Sn and SnO nanomaterial anodes for lithium-ion batteries. J Phys Chem C 120(10):5331–5339Google Scholar
  53. 53.
    Pellicione CJ, Timofeeva EV, Segre CU (2015) In situ X-ray absorption spectroscopy study of the capacity fading mechanism in hybrid Sn3O2(OH)2/graphite battery anode nanomaterials. Chem Mater 27(2):574–580Google Scholar
  54. 54.
    Patridge CJ, Love CT, Swider-Lyons KE, Twigg ME, Ramaker DE (2013) In-situ X-ray absorption spectroscopy analysis of capacity fade in nanoscale-LiCoO2. J Solid State Chem 203:134–144Google Scholar
  55. 55.
    Pelliccione CJ, Li YR, Marschilok AC, Takeuchi KJ, Takeuchi ES (2016) X-ray absorption spectroscopy of lithium insertion and de-insertion in copper birnessite nanoparticle electrodes. Phys Chem Chem Phys 18(4):2959–2967Google Scholar
  56. 56.
    Koo B, Xiong H, Slater MD, Prakapenka VB, Balasubramanian M, Podsiadlo P, Johnson CS, Rajh T, Shevchenko EV (2012) Hollow iron oxide nanoparticles for application in lithium ion batteries. Nano Lett 12(5):2429–2435Google Scholar
  57. 57.
    Koo B, Goli P, Sumant AV, dos Santos Claro PC, Rajh T, Johnson CS, Balandin AA, Shevchenko EV (2014) Toward lithium ion batteries with enhanced thermal conductivity. ACS Nano 8(7):7202–7207Google Scholar
  58. 58.
    Koo B, Chattopadhyay S, Shibata T, Prakapenka VB, Johnson CS, Rajh T, Shevchenko EV (2013) Intercalation of sodium ions into hollow iron oxide nanoparticles. Chem Mater 25(2):245–252Google Scholar
  59. 59.
    Iwasawa Y (1997) Applications of X-ray absorption fine structure to catalysts and model surfaces. J Phys IV 7(C2):67–81Google Scholar
  60. 60.
    Mukerjee S, McGreen J (1999) An in-situ X-ray absorption spectroscopy investigation of the effect of Sn additions to carbon-supported Pt electrocatalysts, part 1. J Electrochem Soc 146(2):600–606Google Scholar
  61. 61.
    Bazin D, Mottet C, Tréglia G, Lynch J (2000) New trends in heterogeneous catalysis processes on metallic clusters from synchrotron radiation and theoretical studies. Appl Surf Sci 164(1–4):140–146Google Scholar
  62. 62.
    Bazin D, Mottet C, Tréglia G (2000) New opportunities to understand heterogeneous catalysis processes on nanoscale bimetallic particles through synchrotron radiation and theoretical studies. Appl Catal A Gen 200:47–54Google Scholar
  63. 63.
    Lee JS, Park ED (2002) In-situ XAFS characterization of supported homogeneous catalysts. Top Catal 18(1–2):67–72Google Scholar
  64. 64.
    Bazin D (2002) Solid state concepts to understand catalysis using nanoscale metallic particles. Top Catal 18(1–2):79–84Google Scholar
  65. 65.
    Grunwaldt JD, Wandeler R, Baiker A (2003) Supercritical fluids in catalysis: opportunities of in-situ spectroscopic studies and monitoring phase behavior. Catal Rev Sci Eng 45(1):1–96Google Scholar
  66. 66.
    Bazin D, Rehr J (2003) Soft X-ray absorption spectroscopy at the cutting edge for nanomaterials used in heterogeneous catalysis: the state of the art. Catal Lett 87(1–2):85–90Google Scholar
  67. 67.
    Bare SR, Ressler T (2009) Chapter 6 characterization of catalysts in reactive atmospheres by X-ray absorption spectroscopy. Adv Catal 52:339–465Google Scholar
  68. 68.
    Grunwaldt JD (2009) Shining X-rays on catalysts at work. J Phys Conf Ser 190(1):012151Google Scholar
  69. 69.
    Andrew J, Lobo RF (2010) Identifying reaction intermediates and catalytic active sites through in situ characterization techniques. Chem Soc Rev 39(12):4783–4793Google Scholar
  70. 70.
    Singh J, Lamberti C, van Bokhoven JA (2010) Advanced X-ray absorption and emission spectroscopy: in situ catalytic studies. Chem Soc Rev 39(12):4754–4766Google Scholar
  71. 71.
    Pascarelli S, Mathon O (2010) Advances in high brilliance energy dispersive X-ray absorption spectroscopy. Phys Chem Chem Phys 12(21):5535–5546Google Scholar
  72. 72.
    Ferri D, Newton MA, Nachtegaal M (2011) Modulation excitation X-ray absorption spectroscopy to probe surface species on heterogeneous catalysts. Top Catal 54(16–18):1070–1078Google Scholar
  73. 73.
    Fechetea I, Wangb Y, Vedrinec JC (2012) The past, present and future of heterogeneous catalysis. Catal Today 189(1):2–27Google Scholar
  74. 74.
    Frenkel AI (2012) Applications of extended X-ray absorption fine-structure spectroscopy to studies of bimetallic nanoparticle catalysts. Chem Soc Rev 41(24):8163–8178Google Scholar
  75. 75.
    Wachs IE (2013) Catalysis science of supported vanadium oxide catalysts. Dalton Trans 42(33):11762–11769Google Scholar
  76. 76.
    Ehteshami SMM, Chan SH (2013) A review of electrocatalysts with enhanced CO tolerance and stability for polymer electrolyte membrane fuel cells. Electrochim Acta 93:334–345Google Scholar
  77. 77.
    Grunwaldt J-D, Wagner JB, Dunin-Barkowski RE (2013) Imaging catalysts at work: a hierarchical approach from the macro-to the meso- and nano-scale. ChemCatChem 5(1):62–80Google Scholar
  78. 78.
    Nemeth L, Bare SR (2014) Science and technology of framework metal containing zeotype catalysts. Adv Catal 57:1–97Google Scholar
  79. 79.
    Garino C, Borfecchia E, Gobetto R, van Bokhoven JA, Lamberti C (2014) Determination of the electronic and structural configuration of coordination compounds by synchrotron-radiation techniques. Coord Chem Rev 277:130–186Google Scholar
  80. 80.
    Tielens F, Bazin D (2015) Operando characterization and DFT modelling of nanospinels: some examples showing the relationship with catalytic activity. Appl Catal A Gen 504:631–641Google Scholar
  81. 81.
    Sherborne GJ, Nguyen BN (2015) Recent XAS studies into homogeneous metal catalyst in fine chemical and pharmaceutical syntheses. Chem Cent J 9(1):37Google Scholar
  82. 82.
    Zhu M, Wachs IE (2015) Iron-based catalysts for the high-temperature water gas shift (HT-WGS) reaction: a review. ACS Catal 6(2):722–732Google Scholar
  83. 83.
    Meneses CT, Flores WH, Sotero AP, Tamura E, Garcia F, Sasaki JM (2006) In situ system for X-ray absorption spectroscopy experiments to investigate nanoparticle crystallization. J Synchrotron Radiat 13(6):468–470Google Scholar
  84. 84.
    Bare SR, Kelly SD, Ravel B, Greenlay N, King L, Mickelson GE (2010) Characterizing industrial catalysts using in situ XAFS under identical conditions. Phys Chem Chem Phys 12(27):7702–7711Google Scholar
  85. 85.
    Nelson RC, Miller JT (2012) An introduction to X-ray absorption spectroscopy and its in situ application to organometallic compounds and homogeneous catalysts. Catal Sci Technol 2(3):461–470Google Scholar
  86. 86.
    Rochet A, Moizan V, Pichon C, Diehl F, Berliet A, Briois V (2011) In situ and operando structural characterization of a Fischer-Tropsch supported cobalt catalyst. Catal Today 171(1):186–191Google Scholar
  87. 87.
    O’Neill BJ, Miller JT, Dietrich PJ, Sollberger FG, Ribeiro FH, Dumesic JA (2014) Operando X-ray absorption spectroscopy studies of sintering for supported copper catalysts during liquid-phase reaction. ChemCatChem 6(9):2493–2496Google Scholar
  88. 88.
    Grunwaldt J-D, Caravati M, Hannemann S, Baiker A (2004) X-ray absorption spectroscopy under reaction conditions: suitability of different reaction cells for combined catalyst characterization and time-resolved studies. Phys Chem Chem Phys 6:3037–3047Google Scholar
  89. 89.
    Kumar A, Miller JT, Mukasyan AS, Wolf EE (2013) In situ XAS and FTIR studies of a multi-component Ni/Fe/Cu catalyst for hydrogen production from ethanol. Appl Catal A Gen 467:593–603Google Scholar
  90. 90.
    Sayah E, Fontaine CL, Briois V, Brouri D, Massiani P (2012) Silver species reduction upon exposure of Ag/Al2O3 catalyst to gaseous ethanol: an in situ quick-XANES study. Catal Today 189(1):155–159Google Scholar
  91. 91.
    Martinelli M, Jocabs G, Graham UM, Shafer WD, Cronauer DC, Kropf AJ, Marshall CL, Khalid S, Visconti CG, Letti L, Davis BH (2015) Water-gas shift: characterization and testing of nanoscale YSZ supported Pt catalysts. Appl Catal A Gen 497:184–197Google Scholar
  92. 92.
    Maclennan A, Banerjee A, Hu Y, Miller JT, Scott RWJ (2013) In situ X-ray absorption spectroscopic analysis of gold–palladium bimetallic nanoparticle catalysts. ACS Catal 3(6):1411–1419Google Scholar
  93. 93.
    Craievich AF (2002) Synchrotron SAXS studies of nanostructured materials and colloidal solutions. A review. Mater Res 5(1):1–11Google Scholar
  94. 94.
    Abécassis B, Testard F, Spalla O, Barboux P (2007) Probing in situ the nucleation and growth of gold nanoparticles by small-angle X-ray scattering. Nano Lett 7(6):1723–1727Google Scholar
  95. 95.
    Susini J, Salome M, Fayward B, Ortega R, Kaulich B (2002) The scanning X-ray microprobe at the ESRF X-ray microscopy beamline. Surf Rev Lett 9(1):203–211Google Scholar
  96. 96.
    Wu J, Shan S, Petkov V, Prasai B, Cronk H, Joseph P, Luo J, Zhong C-J (2015) Composition-structure-activity relationships for palladium-alloyed nanocatalysts in oxygen reduction reaction: an ex-situ/in-situ high energy X-ray diffraction study. ACS Catal 5(9):5317–5327Google Scholar
  97. 97.
    Beyer KA, Zhao H, Borkiewicz OJ, Newton MA, Chupas PJ, Chapman KW (2014) Simultaneous diffuse reflection infrared spectroscopy and X-ray pair distribution function measurements. J Appl Crystallogr 47(1):95–101Google Scholar
  98. 98.
    Chapman KW (2016) Emerging operando and X-ray pair distribution function methods for energy materials developments. MRS Bull 41(3):231–240Google Scholar
  99. 99.
    Oxford SM, Lee PL, Chupas PJ, Chapman KW, Kung MC, Kung HH (2010) Study of supported PtCu and PdAu bimetallic nanoparticles using in-situ X-ray tools. J Phys Chem 114(40):17085–17091Google Scholar
  100. 100.
    Newton MA, van Beek W (2010) Combining synchrotron-based X-ray techniques with vibrational spectroscopies for the in situ study of heterogeneous catalysts: a view from a bridge. Chem Soc Rev 39(12):4845–4863Google Scholar
  101. 101.
    Ehrlich SN, Henson JC, Camara AL, Bariio L, Estralla M, Zhou G, Si R, Khalid S, Wang Q (2011) Combined XRD and XAS. Nucl Inst Methods Phys Res A 649(1):213–215Google Scholar
  102. 102.
    Gallagher JR, Li T, Zhao H, Liu J, Lei Y, Zhang X, Ren Y, Elam JW, Meyer RJ, Winans RE, Miller JT (2014) In situ diffraction of highly dispersed supported platinum nanoparticle. Catal Sci Technol 4(9):3053–3063Google Scholar
  103. 103.
    Gallagher JR, Childers DJ, Zhao H, Winans RE, Meyer RJ, Miller JT (2015) Structural evolution of an intermetallic Pd-Zn catalyst selective for propane dehydrogenation. Phys Chem Chem Phys 17(42):28144–28153Google Scholar
  104. 104.
    Muñoz FF, Cabezas MD, Acuña LM, Leyva AG, Baker RT, Fuentes RO (2011) Structural properties and reduction behavior of novel nanostructured Pd/gadolinia-doped ceria catalysts with tubular morphology. J Phys Chem C 115(17):8744–8752Google Scholar
  105. 105.
    Sasaki K, Kuttiyiel KA, Barrio L, Su D, Frenkel AI, Marinkovic N, Mahajan D, Adzic RR (2011) Carbon-supported IrNi core-shell nanoparticles: synthesis, characterization, and catalytic activity. J Phys Chem C 115(20):9894–9902Google Scholar
  106. 106.
    Keating J, Sankar G, Hyde TI, Kohara S, Ohara K (2013) Elucidation of structure and nature of the PdO–Pd transformation using in situ PDF and XAS techniques. Phys Chem Chem Phys 15(22):8555–8565Google Scholar
  107. 107.
    Kan Y, Hu Y, Croy J, Ren Y, Sun C-J, Heald SM, Bareño J, Bloom I, Chen Z (2014) Formation of Li2MnO3 investigated by in situ synchrotron probes. J Power Sources 266:341–346Google Scholar
  108. 108.
    Zhang K, Zhao Z, Wu Z, Zhou Y (2015) Synthesis and detection the oxidization of Co cores of Co@SiO2 core-shell nanoparticles by in situ XRD and EXAFS. Nanoscale Res Lett 10(1):37Google Scholar
  109. 109.
    Cormary B, Li T, Liakakos N, Peres L, Fazzini P-F, Blon T, Respaud M, Kropf AJ, Chaudret B, Miller JT, Mader EA, Soulantica K (2016) Concerted growth and ordering of cobalt nanorod arrays as revealed by tandem in situ SAXS-XAS studies. J Am Chem Soc 138(27):8422–8431Google Scholar
  110. 110.
    Penfold TJ, Milne CJ, Chergui M (2013) Recent advances in ultrafast X-ray spectroscopy of solutions. In: Rice SA, Dinner AR (eds) Advances in chemical physics, 2nd edn. Wiley, Hoboken, pp 1–41Google Scholar
  111. 111.
    Borfecchia E, Garino C, Salassa L, Lamberti C (2013) Synchrotron ultrafast techniques for photoactive transition metal complexes. Phil Trans R Soc A 371:20120132. Scholar
  112. 112.
    Ortega R (2012) X-ray absorption spectroscopy of biological samples. A tutorial. J Anal At Spectrom 27(12):2054–2065Google Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Soma Chattopadhyay
    • 1
  • Soon Gu Kwon
    • 2
  • Elena V. Shevchenko
    • 3
  • Jeffrey T. Miller
    • 4
  • Steve M. Heald
    • 5
  1. 1.Elgin Community CollegeElginUSA
  2. 2.Center for Nanoparticle ResearchInstitute for Basic Science and Seoul National UniversitySeoulRepublic of Korea
  3. 3.Nanoscience and Technology divisionArgonne National LaboratoryArgonneUSA
  4. 4.School of Chemical EngineeringPurdue UniversityWest LafayetteUSA
  5. 5.Advanced Photon SourceArgonne National LaboratoryArgonneUSA

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