Revealing Complexity of Nanoparticle Synthesis in Solution by in Situ Hard X-ray Spectroscopy - Today and beyond

Chemistry of Materials

Volumn 28, Issue 8, 2016, Pages 2478-2490

  Koziej, Dorota ^a  

^a ETH ZURICH   (Switzerland)

Author keywords

[No Author keywords available]

Indexed keywords

DATA ACQUISITION; NANOPARTICLES; SPECTROSCOPIC ANALYSIS; X RAY SPECTROSCOPY;

COLLOIDAL NANOPARTICLES; CONCENTRATION GRADIENTS; HARD X-RAY SPECTROSCOPY; MULTI-COMPONENT STRUCTURES; NANOPARTICLE SYNTHESIS; RAPID DATA ACQUISITION; SPECTROSCOPIC STUDIES; STRUCTURAL INHOMOGENEITIES;

SYNTHESIS (CHEMICAL);

EID: 84969257803     PISSN: 08974756     EISSN: 15205002     Source Type: Journal    
DOI: 10.1021/acs.chemmater.6b00486     Document Type: Article

References (137)

1. Kovalenko, M. V.; Manna, L.; Cabot, A.; Hens, Z.; Talapin, D. V.; Kagan, C. R.; Klimov, V. I.; Rogach, A. L.; Reiss, P.; Milliron, D. J.; Guyot-Sionnnest, P.; Konstantatos, G.; Parak, W. J.; Hyeon, T.; Korgel, B. A.; Murray, C. B.; Heiss, W. Prospects of Nanoscience with Nanocrystals ACS Nano 2015, 9, 1012 10.1021/nn506223h
2. Koziej, D.; Lauria, A.; Niederberger, M. 25th Anniversary Article: Metal Oxide Particles in Materials Science: Addressing All Length Scales Adv. Mater. 2014, 26, 235 10.1002/adma.201303161
3. Boissiere, C.; Grosso, D.; Chaumonnot, A.; Nicole, L.; Sanchez, C. Aerosol Route to Functional Nanostructured Inorganic and Hybrid Porous Materials Adv. Mater. 2011, 23, 599 10.1002/adma.201001410
4. Cargnello, M.; Agarwal, R.; Klein, D. R.; Diroll, B. T.; Agarwal, R.; Murray, C. B. Uniform Bimetallic Nanocrystals by High-Temperature Seed-Mediated Colloidal Synthesis and Their Catalytic Properties for Semiconducting Nanowire Growth Chem. Mater. 2015, 27, 5833 10.1021/acs.chemmater.5b02900
5. Cargnello, M.; Johnston-Peck, A. C.; Diroll, B. T.; Wong, E.; Datta, B.; Damodhar, D.; Doan-Nguyen, V. V. T.; Herzing, A. A.; Kagan, C. R.; Murray, C. B. Substitutional doping in nanocrystal superlattices Nature 2015, 524, 450 10.1038/nature14872
6. Sahu, A.; Kang, M. S.; Kompch, A.; Notthoff, C.; Wills, A. W.; Deng, D.; Winterer, M.; Frisbie, C. D.; Norris, D. J. Electronic Impurity Doping in CdSe Nanocrystals Nano Lett. 2012, 12, 2587 10.1021/nl300880g
7. Kwon, S. G.; Hyeon, T. Formation Mechanisms of Uniform Nanocrystals via Hot-Injection and Heat-Up Methods Small 2011, 7, 2685 10.1002/smll.201002022
8. Bau, J. A.; Li, P.; Marenco, A. J.; Trudel, S.; Olsen, B. C.; Luber, E. J.; Buriak, J. M. Nickel/Iron Oxide Nanocrystals with a Nonequilibrium Phase: Controlling Size, Shape, and Composition Chem. Mater. 2014, 26, 4796 10.1021/cm501881a
9. Liu, H. Q.; Li, L. Y.; Scofield, M. E.; Wong, S. S. Research Update: Synthesis, properties, and applications of ultrathin metallic nanowires and associated heterostructures APL Mater. 2015, 3, 080701 10.1063/1.4927797
10. Zhang, J. T.; Tang, Y.; Lee, K.; Ouyang, M. Nonepitaxial Growth of Hybrid Core-Shell Nanostructures with Large Lattice Mismatches Science 2010, 327, 1634 10.1126/science.1184769
11. Jensen, K. M. O.; Tyrsted, C.; Bremholm, M.; Iversen, B. B. In Situ Studies of Solvothermal Synthesis of Energy Materials ChemSusChem 2014, 7, 1594 10.1002/cssc.201301042
12. Ingham, B. X-ray scattering characterisation of nanoparticles Crystallogr. Rev. 2015, 21, 229 10.1080/0889311X.2015.1024114
13. Billinge, S. J. L.; Levin, I. The problem with determining atomic structure at the nanoscale Science 2007, 316, 561 10.1126/science.1135080
14. Becker, J.; Bremholm, M.; Tyrsted, C.; Pauw, B.; Jensen, K. M. O.; Eltzholt, J.; Christensen, M.; Iversen, B. B. Experimental setup for in situ X-ray SAXS/WAXS/PDF studies of the formation and growth of nanoparticles in near- and supercritical fluids J. Appl. Crystallogr. 2010, 43, 729 10.1107/S0021889810014688
15. Bras, W.; Koizumi, S.; Terrill, N. J. Beyond simple small-angle X-ray scattering: developments in online complementary techniques and sample environments IUCrJ 2014, 1, 478 10.1107/S2052252514019198
16. Polte, J.; Erler, R.; Thunemann, A. F.; Sokolov, S.; Ahner, T. T.; Rademann, K.; Emmerling, F.; Kraehnert, R. Nucleation and Growth of Gold Nanoparticles Studied via in situ Small Angle X-ray Scattering at Millisecond Time Resolution ACS Nano 2010, 4, 1076 10.1021/nn901499c
17. Abecassis, B.; Bouet, C.; Garnero, C.; Constantin, D.; Lequeux, N.; Ithurria, S.; Dubertret, B.; Pauw, B. R.; Pontoni, D. Real-Time in Situ Probing of High-Temperature Quantum Dots Solution Synthesis Nano Lett. 2015, 15, 2620 10.1021/acs.nanolett.5b00199
18. Wang, J. A.; Winans, R. E.; Anderson, S. L.; Seifert, S.; Lee, B.; Chupas, P. J.; Ren, Y.; Lee, S.; Liu, Y. Z. In Situ Small-Angle X-ray Scattering from Pd Nanoparticles Formed by Thermal Decomposition of Organo-Pd Catalyst Precursors Dissolved in Hydrocarbons J. Phys. Chem. C 2013, 117, 22627 10.1021/jp402513z
19. Petkov, V. Nanostructure by high-energy X-ray diffraction Mater. Today 2008, 11, 28 10.1016/S1369-7021(08)70236-0
20. Billinge, S. J. L. Nanoscale structural order from the atomic pair distribution function (PDF): There's plenty of room in the middle J. Solid State Chem. 2008, 181, 1695 10.1016/j.jssc.2008.06.046
21. Petkov, V.; Bedford, N.; Knecht, M. R.; Weir, M. G.; Crooks, R. M.; Tang, W.; Henkelman, G.; Frenkel, A. Periodicity and atomic ordering in nanosized particles of crystals J. Phys. Chem. C 2008, 112, 8907 10.1021/jp801195c
22. Newton, M. A.; Chapman, K. W.; Thompsett, D.; Chupas, P. J. Chasing Changing Nanoparticles with Time-Resolved Pair Distribution Function Methods J. Am. Chem. Soc. 2012, 134, 5036 10.1021/ja2114163
23. Proffen, T.; Billinge, S. J. L.; Egami, T.; Louca, D. Structural analysis of complex materials using the atomic pair distribution function-a practical guide Z. Kristallogr.-Cryst. Mater. 2003, 218, 132 10.1524/zkri.218.2.132.20664
24. Egami, T.; Billinge, S. J. L. Underneath the Bragg peaks: structural analysis of complex materials; Pergamon: Oxford, 2003; Vol. 7.
25. Chupas, P. J.; Chapman, K. W.; Jennings, G.; Lee, P. L.; Grey, C. P. Watching nanoparticles grow: The mechanism and kinetics for the formation of TiO2-supported platinum nanoparticles J. Am. Chem. Soc. 2007, 129, 13822 10.1021/ja076437p
26. Chupas, P. J.; Qiu, X. Y.; Hanson, J. C.; Lee, P. L.; Grey, C. P.; Billinge, S. J. L. Rapid-acquisition pair distribution function (RA-PDF) analysis J. Appl. Crystallogr. 2003, 36, 1342 10.1107/S0021889803017564
27. Young, C. A.; Goodwin, A. L. Applications of pair distribution function methods to contemporary problems in materials chemistry J. Mater. Chem. 2011, 21, 6464 10.1039/c0jm04415f
28. Farrow, C. L.; Juhas, P.; Liu, J. W.; Bryndin, D.; Bozin, E. S.; Bloch, J.; Proffen, T.; Billinge, S. J. L. PDFfit2 and PDFgui: computer programs for studying nanostructure in crystals J. Phys.: Condens. Matter 2007, 19, 335219 10.1088/0953-8984/19/33/335219
29. Sun, Y. G.; Ren, Y. In Situ Synchrotron X-Ray Techniques for Real-Time Probing of Colloidal Nanoparticle Synthesis Part. & Part. Syst. Charact. 2013, 30, 399 10.1002/ppsc.201300033
30. Lamer, V. K.; Dinegar, R. H. Theory, Production and Mechanism of Formation of Monodispersed Hydrosols J. Am. Chem. Soc. 1950, 72, 4847 10.1021/ja01167a001
31. Gebauer, D.; Colfen, H. Prenucleation clusters and non-classical nucleation Nano Today 2011, 6, 564 10.1016/j.nantod.2011.10.005
32. Thanh, N. T. K.; Maclean, N.; Mahiddine, S. Mechanisms of Nucleation and Growth of Nanoparticles in Solution Chem. Rev. 2014, 114, 7610 10.1021/cr400544s
33. Lee, E. J. H.; Ribeiro, C.; Longo, E.; Leite, E. R. Oriented attachment: An effective mechanism in the formation of anisotropic nanocrystals J. Phys. Chem. B 2005, 109, 20842 10.1021/jp0532115
34. Zhang, H. Z.; De Yoreo, J. J.; Banfield, J. F. A Unified Description of Attachment-Based Crystal Growth ACS Nano 2014, 8, 6526 10.1021/nn503145w
35. Moore, D. T.; Sai, H.; Tan, K. W.; Smilgies, D. M.; Zhang, W.; Snaith, H. J.; Wiesner, U.; Estroff, L. A. Crystallization Kinetics of Organic-Inorganic Trihalide Perovskites and the Role of the Lead Anion in Crystal Growth J. Am. Chem. Soc. 2015, 137, 2350 10.1021/ja512117e
36. Vreeland, E. C.; Watt, J.; Schober, G. B.; Hance, B. G.; Austin, M. J.; Price, A. D.; Fellows, B. D.; Monson, T. C.; Hudak, N. S.; Maldonado-Camargo, L.; Bohorquez, A. C.; Rinaldi, C.; Huber, D. L. Enhanced Nanoparticle Size Control by Extending LaMer's Mechanism Chem. Mater. 2015, 27, 6059 10.1021/acs.chemmater.5b02510
37. Garnweitner, G.; Gebauer, D.; Niederberger, M. Fundamentals of nanocrystal formation CrystEngComm 2015, 17, 6778 10.1039/C5CE90141C
38. Wuithschick, M.; Birnbaum, A.; Witte, S.; Sztucki, M.; Vainio, U.; Pinna, N.; Rademann, K.; Emmerling, F.; Kraehnert, R.; Polte, J. Turkevich in New Robes: Key Questions Answered for the Most Common Gold Nanoparticle Synthesis ACS Nano 2015, 9, 7052 10.1021/acsnano.5b01579
39. Sun, C. C.; Sun, W. H.; Price, S.; Hughes, C.; Ter Horst, J.; Veesler, S.; Lewtas, K.; Myerson, A.; Pan, H. H.; Coquerel, G.; van den Ende, J.; Meekes, H.; Mazzotti, M.; Rosbottom, I.; Taulelle, F.; Black, S.; Mackenzie, A.; Janbon, S.; Vekilov, P.; Threlfall, T.; Turner, T.; Back, K.; Cuppen, H.; Toroz, D.; Sefcik, J.; Lovelock, J.; Hammond, R.; Candoni, N.; Simone, E.; Ward, M.; Bertran, C. A.; Vetter, T.; Sear, R.; De Yoreo, J.; Davey, R.; Anwar, J.; Santiso, E.; Wu, D. T.; Roberts, K.; Peters, B.; Schroeder, S.; Jones, F.; Rasmuson, A.; Colfen, H.; Zeglinski, J.; Salvalaglio, M. Solvent and additive interactions as determinants in the nucleation pathway: general discussion Faraday Discuss. 2015, 179, 383 10.1039/C5FD90038G
40. Staniuk, M.; Zindel, D.; van Beek, W.; Hirsch, O.; Kranzlin, N.; Niederberger, M.; Koziej, D. Matching the organic and inorganic counterparts during nucleation and growth of copper-based nanoparticles-in situ spectroscopic studies CrystEngComm 2015, 17, 6962 10.1039/C5CE00454C
41. van Embden, J.; Chesman, A. S. R.; Jasieniak, J. J. The Heat-Up Synthesis of Colloidal Nanocrystals Chem. Mater. 2015, 27, 2246 10.1021/cm5028964
42. Garnweitner, G.; Niederberger, M. Organic chemistry in inorganic nanomaterials synthesis J. Mater. Chem. 2008, 18, 1171 10.1039/B713775C
43. Alayoglu, S.; Zavalij, P.; Eichhorn, B.; Wang, Q.; Frenkel, A. I.; Chupas, P. Structural and Architectural Evaluation of Bimetallic Nanoparticles: A Case Study of Pt-Ru Core-Shell and Alloy Nanoparticles ACS Nano 2009, 3, 3127 10.1021/nn900242v
44. Peng, X. G.; Manna, L.; Yang, W. D.; Wickham, J.; Scher, E.; Kadavanich, A.; Alivisatos, A. P. Shape control of CdSe nanocrystals Nature 2000, 404, 59 10.1038/35003535
45. Patra, B. K.; Sarkar, S.; Guria, A. K.; Pradhan, N. Monodisperse SnS Nanocrystals: In Just 5 Seconds J. Phys. Chem. Lett. 2013, 4, 3929 10.1021/jz402294x
46. Bilecka, I.; Djerdj, I.; Niederberger, M. One-minute synthesis of crystalline binary and ternary metal oxide nanoparticles Chem. Commun. 2008, 886 10.1039/B717334B
47. Bilecka, I.; Niederberger, M. Microwave chemistry for inorganic nanomaterials synthesis Nanoscale 2010, 2, 1358 10.1039/b9nr00377k
48. Di Carlo, L.; Conte, D. E.; Kemnitz, E.; Pinna, N. Microwave-assisted fluorolytic sol-gel route to iron fluoride nanoparticles for Li-Ion batteries Chem. Commun. 2014, 50, 460 10.1039/C3CC47413E
49. Phillips, T. W.; Lignos, I. G.; Maceiczyk, R. M.; deMello, A. J.; deMello, J. C. Nanocrystal synthesis in microfluidic reactors: where next? Lab Chip 2014, 14, 3172 10.1039/C4LC00429A
50. Koziej, D.; Floryan, C.; Sperling, R. A.; Ehrlicher, A. J.; Issadore, D.; Westervelt, R.; Weitz, D. A. Microwave dielectric heating of non-aqueous droplets in a microfluidic device for nanoparticle synthesis Nanoscale 2013, 5, 5468 10.1039/c3nr00500c
51. Karim, A. M.; Al Hasan, N.; Ivanov, S.; Siefert, S.; Kelly, R. T.; Hallfors, N. G.; Benavidez, A.; Kovarik, L.; Jenkins, A.; Winans, R. E.; Datye, A. K. Synthesis of 1 nm Pd Nanoparticles in a Microfluidic Reactor: Insights from in Situ X-ray Absorption Fine Structure Spectroscopy and Small-Angle X-ray Scattering J. Phys. Chem. C 2015, 119, 13257 10.1021/acs.jpcc.5b01681
52. Chakrabarty, A.; Marre, S.; Landis, R. F.; Rotello, V. M.; Maitra, U.; Del Guerzo, A.; Aymonier, C. Continuous synthesis of high quality CdSe quantum dots in supercritical fluids J. Mater. Chem. C 2015, 3, 7561 10.1039/C5TC01115A
53. Marre, S.; Jensen, K. F. Synthesis of micro and nanostructures in microfluidic systems Chem. Soc. Rev. 2010, 39, 1183 10.1039/b821324k
54. Pascu, O.; Marre, S.; Aymonier, C.; Roig, A. Ultrafast and continuous synthesis of crystalline ferrite nanoparticles in supercritical ethanol Nanoscale 2013, 5, 2126 10.1039/c3nr33501a
55. Frenkel, A. I.; Khalid, S.; Hanson, J. C.; Nachtegaal, M. Qexafs in Catalysis Research: Principles, Data Analysis, and Applications In-Situ Characterization of Heterogeneous Catalysts 2013, 23 10.1002/9781118355923.ch1
56. Kantor, I.; Labiche, J. C.; Collet, E.; Siron, L.; Thevenin, J. J.; Ponchut, C.; Borrel, J.; Mairs, T.; Marini, C.; Strohm, C.; Mathon, O.; Pascarelli, S. A new detector for sub-millisecond EXAFS spectroscopy at the European Synchrotron Radiation Facility J. Synchrotron Radiat. 2014, 21, 1240 10.1107/S1600577514014805
57. Prestipino, C.; Mathon, O.; Hino, R.; Beteva, A.; Pascarelli, S. Quick-EXAFS implementation on the general purpose EXAFS beamline at ESRF J. Synchrotron Radiat. 2011, 18, 176 10.1107/S0909049510046546
58. Pettifer, R. F.; Mathon, O.; Pascarelli, S.; Cooke, M. D.; Gibbs, M. R. J. Measurement of femtometre-scale atomic displacements by X-ray absorption spectroscopy Nature 2005, 435, 78 10.1038/nature03516
59. Frenkel, A. I. Applications of extended X-ray absorption fine-structure spectroscopy to studies of bimetallic nanoparticle catalysts Chem. Soc. Rev. 2012, 41, 8163 10.1039/c2cs35174a
60. Frenkel, A. I.; Wang, Q.; Sanchez, S. I.; Small, M. W.; Nuzzo, R. G. Short range order in bimetallic nanoalloys: An extended X-ray absorption fine structure study J. Chem. Phys. 2013, 138, 064202 10.1063/1.4790509
61. Paun, C.; Safonova, O. V.; Szlachetko, J.; Abdala, P. M.; Nachtegaal, M.; Sa, J.; Kleymenov, E.; Cervellino, A.; Krumeich, F.; van Bokhoven, J. A. Polyhedral CeO2 Nanoparticles: Size-Dependent Geometrical and Electronic Structure J. Phys. Chem. C 2012, 116, 7312 10.1021/jp300342b
62. Beale, A. M.; Weckhuysen, B. M. EXAFS as a tool to interrogate the size and shape of mono and bimetallic catalyst nanoparticles Phys. Chem. Chem. Phys. 2010, 12, 5562 10.1039/b925206a
63. Chill, S. T.; Anderson, R. M.; Yancey, D. F.; Frenkel, A. I.; Crooks, R. M.; Henkelman, G. Probing the Limits of Conventional Extended X-ray Absorption Fine Structure Analysis Using Thiolated Gold Nanoparticles ACS Nano 2015, 9, 4036 10.1021/acsnano.5b00090
64. Rehr, J. J.; Kas, J. J.; Vila, F. D.; Prange, M. P.; Jorissen, K. Parameter-free calculations of X-ray spectra with FEFF9 Phys. Chem. Chem. Phys. 2010, 12, 5503 10.1039/b926434e
65. Hirsch, O.; Kvashnina, K. O.; Luo, L.; Süess, M. J.; Glatzel, P.; Koziej, D. High-energy resolution X-ray absorption and emission spectroscopy reveals insight into unique selectivity of La-based nanoparticles for CO2 Proc. Natl. Acad. Sci. U. S. A. 2015, 112, 15803 10.1073/pnas.1516192113
66. Szlachetko, J.; Sa, J. Rational design of oxynitride materials: From theory to experiment CrystEngComm 2013, 15, 2583 10.1039/c3ce26909d
67. Szlachetko, J.; Nachtegaal, M.; de Boni, E.; Willimann, M.; Safonova, O.; Sa, J.; Smolentsev, G.; Szlachetko, M.; van Bokhoven, J. A.; Dousse, J. C.; Hoszowska, J.; Kayser, Y.; Jagodzinski, P.; Bergamaschi, A.; Schmitt, B.; David, C.; Lucke, A. A von Hamos x-ray spectrometer based on a segmented-type diffraction crystal for single-shot x-ray emission spectroscopy and time-resolved resonant inelastic x-ray scattering studies Rev. Sci. Instrum. 2012, 83, 103105 10.1063/1.4756691
68. Gallo, E.; Glatzel, P. Valence to Core X-ray Emission Spectroscopy Adv. Mater. 2014, 26, 7730 10.1002/adma.201304994
69. Glatzel, P.; Weng, T. C.; Kvashnina, K.; Swarbrick, J.; Sikora, M.; Gallo, E.; Smolentsev, N.; Mori, R. A. Reflections on hard X-ray photon-in/photon-out spectroscopy for electronic structure studies J. Electron Spectrosc. Relat. Phenom. 2013, 188, 17 10.1016/j.elspec.2012.09.004
70. Bauer, M. HERFD-XAS and valence-to-core-XES: new tools to push the limits in research with hard X-rays? Phys. Chem. Chem. Phys. 2014, 16, 13827 10.1039/C4CP00904E
71. Sa, J.; Kayser, Y.; Milne, C. J.; Fernandes, D. L. A.; Szlachetko, J. Temperature-programmed reduction of NiO nanoparticles followed by time-resolved RIXS Phys. Chem. Chem. Phys. 2014, 16, 7692 10.1039/c3cp54622e
72. Szlachetko, J.; Michalow-Mauke, K.; Nachtegaal, M.; Sa, J. Determination of conduction and valence band electronic structure of anatase and rutile TiO2 J. Chem. Sci. 2014, 126, 511 10.1007/s12039-014-0584-1
73. Boubnov, A.; Carvalho, H. W. P.; Doronkin, D. E.; Gunter, T.; Gallo, E.; Atkins, A. J.; Jacob, C. R.; Grunwaldt, J. D. Selective Catalytic Reduction of NO Over Fe-ZSM-5: Mechanistic Insights by Operando HERFD-XANES and Valence-to-Core X-ray Emission Spectroscopy J. Am. Chem. Soc. 2014, 136, 13006 10.1021/ja5062505
74. Johann, H. H. The production-aperture x-ray spectra with the help of concave crystals Eur. Phys. J. A 1931, 69, 185 10.1007/BF01798121
75. von Hamos, L. Röntgenspektroskopie und Abbildung mittels gekrümmter Kristallreflektoren Naturwissenschaften 1932, 20, 705 10.1007/BF01494468
76. Thomas, R.; Kas, J.; Glatzel, P.; Al Samarai, M.; de Groot, F. M. F.; Mori, R. A.; Kavcic, M.; Zitnik, M.; Bucar, K.; Rehr, J. J.; Tromp, M. Resonant Inelastic X-ray Scattering of Molybdenum Oxides and Sulfides J. Phys. Chem. C 2015, 119, 2419 10.1021/jp509376q
77. Soininen, J. A.; Ankudinov, A. L.; Rehr, J. J. Inelastic scattering from core electrons: A multiple scattering approach Phys. Rev. B: Condens. Matter Mater. Phys. 2005, 72, 045136 10.1103/PhysRevB.72.045136
78. Rehr, J. J.; Ankudinov, A. L. Progress in the theory and interpretation of XANES Coordin Coord. Chem. Rev. 2005, 249, 131 10.1016/j.ccr.2004.02.014
79. Kas, J. J.; Rehr, J. J.; Soininen, J. A.; Glatzel, P. Real-space Green's function approach to resonant inelastic x-ray scattering Phys. Rev. B: Condens. Matter Mater. Phys. 2011, 83, 235114 10.1103/PhysRevB.83.235114
80. Filipponi, A.; DiCicco, A.; Natoli, C. R. X-ray-absorption spectroscopy and n-body distribution functions in condensed matter 0.1. Theory Phys. Rev. B: Condens. Matter Mater. Phys. 1995, 52, 15122 10.1103/PhysRevB.52.15122
81. Joly, Y.; Bunau, O.; Lorenzo, J. E.; Galera, R. M.; Grenier, S.; Thompson, B. Self-consistency, spin-orbit and other advances in the FDMNES code to simulate XANES and RXD experiments J. Phys. Conf. Ser. 2009, 190, 012007 10.1088/1742-6596/190/1/012007
82. Schwarz, K.; Blaha, P.; Trickey, S. B. Electronic structure of solids with WIEN2k Mol. Phys. 2010, 108, 3147 10.1080/00268976.2010.506451
83. Bordiga, S.; Groppo, E.; Agostini, G.; van Bokhoven, J. A.; Lamberti, C. Reactivity of Surface Species in Heterogeneous Catalysts Probed by In Situ X-ray Absorption Techniques Chem. Rev. 2013, 113, 1736 10.1021/cr2000898
84. Kavcic, M.; Zitnik, M.; Bucar, K.; Mihelic, A.; Marolt, B.; Szlachetko, J.; Glatzel, P.; Kvashnina, K. Hard x-ray absorption spectroscopy for pulsed sources Phys. Rev. B: Condens. Matter Mater. Phys. 2013, 87, 075106 10.1103/PhysRevB.87.075106
85. Reinhardt, F.; Beckhoff, B.; Eba, H.; Kanngiesser, B.; Kolbe, M.; Mizusawa, M.; Muller, M.; Pollakowski, B.; Sakurai, K.; Ulm, G. Evaluation of High-Resolution X-ray Absorption and Emission Spectroscopy for the Chemical Speciation of Binary Titanium Compounds Anal. Chem. 2009, 81, 1770 10.1021/ac8018069
86. Hubner, M.; Koziej, D.; Bauer, M.; Barsan, N.; Kvashnina, K.; Rossell, M. D.; Weimar, U.; Grunwaldt, J. D. The Structure and Behavior of Platinum in SnO2-Based Sensors under Working Conditions Angew. Chem., Int. Ed. 2011, 50, 2841 10.1002/anie.201004499
87. Kuhn, T. J.; Hormes, J.; Matoussevitch, N.; Bonnemann, H.; Glatzel, P. Site-Selective High-Resolution X-ray Absorption Spectroscopy and High-Resolution X-ray Emission Spectroscopy of Cobalt Nanoparticles Inorg. Chem. 2014, 53, 8367 10.1021/ic5000183
88. Pollock, C. J.; DeBeer, S. Valence-to-Core X-ray Emission Spectroscopy: A Sensitive Probe of the Nature of a Bound Ligand J. Am. Chem. Soc. 2011, 133, 5594 10.1021/ja200560z
89. Pollock, C. J.; DeBeer, S. Insights into the Geometric and Electronic Structure of Transition Metal Centers from Valence-to-Core X-ray Emission Spectroscopy Acc. Chem. Res. 2015, 48, 2967 10.1021/acs.accounts.5b00309
90. Hall, E. R.; Pollock, C. J.; Bendix, J.; Collins, T. J.; Glatzel, P.; DeBeer, S. Valence-to-Core-Detected X-ray Absorption Spectroscopy: Targeting Ligand Selectivity J. Am. Chem. Soc. 2014, 136, 10076 10.1021/ja504206y
91. Giordanino, F.; Borfecchia, E.; Lomachenko, K. A.; Lazzarini, A.; Agostini, G.; Gallo, E.; Soldatov, A. V.; Beato, P.; Bordiga, S.; Lamberti, C. Interaction of NH3 with Cu-SSZ-13 Catalyst: A Complementary FTIR, XANES, and XES Study J. Phys. Chem. Lett. 2014, 5, 1552 10.1021/jz500241m
92. Groppo, E.; Gallo, E.; Seenivasan, K.; Lomachenko, K. A.; Sommazzi, A.; Bordiga, S.; Glatzel, P.; van Silfhout, R.; Kachatkou, A.; Bras, W.; Lamberti, C. XAS and XES Techniques Shed Light on the Dark Side of Ziegler-Natta Catalysts: Active-Site Generation ChemCatChem 2015, 7, 1432 10.1002/cctc.201402989
93. March, A. M.; Assefa, T. A.; Bressler, C.; Doumy, G.; Galler, A.; Gawelda, W.; Kanter, E. P.; Nemeth, Z.; Papai, M.; Southworth, S. H.; Young, L.; Vanko, G. Feasibility of Valence-to-Core X-ray Emission Spectroscopy for Tracking Transient Species J. Phys. Chem. C 2015, 119, 14571 10.1021/jp511838q
94. Zhang, W. K.; Alonso-Mori, R.; Bergmann, U.; Bressler, C.; Chollet, M.; Galler, A.; Gawelda, W.; Hadt, R. G.; Hartsock, R. W.; Kroll, T.; Kjaer, K. S.; Kubicek, K.; Lemke, H. T.; Liang, H. Y. W.; Meyer, D. A.; Nielsen, M. M.; Purser, C.; Robinson, J. S.; Solomon, E. I.; Sun, Z.; Sokaras, D.; van Driel, T. B.; Vanko, G.; Weng, T. C.; Zhu, D. L.; Gaffney, K. J. Tracking excited-state charge and spin dynamics in iron coordination complexes Nature 2014, 509, 345 10.1038/nature13252
95. Szlachetko, J.; Sa, J.; Nachtegaal, M.; Hartfelder, U.; Dousse, J. C.; Hoszowska, J.; Fernandes, D. L. A.; Shi, H. Q.; Stampfl, C. Real Time Determination of the Electronic Structure of Unstable Reaction Intermediates during Au2O3 Reduction J. Phys. Chem. Lett. 2014, 5, 80 10.1021/jz402309s
96. Bordage, A.; Trannoy, V.; Proux, O.; Vitoux, H.; Moulin, R.; Bleuzen, A. In situ site-selective transition metal K-edge XAS: a powerful probe of the transformation of mixed-valence compounds Phys. Chem. Chem. Phys. 2015, 17, 17260 10.1039/C5CP02591E
97. Stotzel, J.; Lutzenkirchen-Hecht, D.; Frahm, R.; Santilli, C. V.; Pulcinelli, S. H.; Kaminski, R.; Fonda, E.; Villain, F.; Briois, V. QEXAFS and UV/Vis Simultaneous Monitoring of the TiO2-Nanoparticles Formation by Hydrolytic Sol-Gel Route J. Phys. Chem. C 2010, 114, 6228 10.1021/jp9105019
98. Kranzlin, N.; Staniuk, M.; Heiligtag, F. J.; Luo, L.; Emerich, H.; van Beek, W.; Niederberger, M.; Koziej, D. Rationale for the crystallization of titania polymorphs in solution Nanoscale 2014, 6, 14716 10.1039/C4NR04346D
99. Cafun, J. D.; Kvashnina, K. O.; Casals, E.; Puntes, V. F.; Glatzel, P. Absence of Ce3+ Sites in Chemically Active Colloidal Ceria Nanoparticles ACS Nano 2013, 7, 10726 10.1021/nn403542p
100. Booth, S. G.; Uehara, A.; Chang, S. Y.; Mosselmans, J. F. W.; Schroeder, S. L. M.; Dryfe, R. A. W. Gold Deposition at a Free-Standing Liquid/Liquid Interface: Evidence for the Formation of Au(I) by Microfocus X-ray Spectroscopy (mu XRF and mu XAFS) and Cyclic Voltammetry J. Phys. Chem. C 2015, 119, 16785 10.1021/acs.jpcc.5b05127
101. Grunwaldt, J. D.; Ramin, M.; Rohr, M.; Michailovski, A.; Patzke, G. R.; Baiker, A. Rev. Sci. Instrum. 2005, 76, 054104 10.1063/1.1914787
102. Staniuk, M.; Hirsch, O.; Kranzlin, N.; Bohlen, R.; van Beek, W.; Abdala, P. M.; Koziej, D. Puzzling Mechanism behind a Simple Synthesis of Cobalt and Cobalt Oxide Nanoparticles: In Situ Synchrotron X-ray Absorption and Diffraction Studies Chem. Mater. 2014, 26, 2086 10.1021/cm500090r
103. Chan, E. M.; Marcus, M. A.; Fakra, S.; ElNaggar, M.; Mathies, R. A.; Alivisatos, A. P. Millisecond kinetics of nanocrystal cation exchange using microfluidic X-ray absorption spectroscopy J. Phys. Chem. A 2007, 111, 12210 10.1021/jp073474u
104. Oyanagi, H.; Sun, Z. H.; Jiang, Y.; Uehara, M.; Nakamura, H.; Yamashita, K.; Zhang, L.; Lee, C.; Fukano, A.; Maeda, H. In situ XAFS experiments using a microfluidic cell: application to initial growth of CdSe nanocrystals J. Synchrotron Radiat. 2011, 18, 272 10.1107/S0909049510050545
105. Sun, Z. H.; Oyanagi, H.; Uehara, M.; Nakamura, H.; Yamashita, K.; Fukano, A.; Maeda, H. Study on Initial Kinetics of CdSe Nanocrystals by a Combination of in Situ X-ray Absorption Fine Structure and Microfluidic Reactor J. Phys. Chem. C 2009, 113, 18608 10.1021/jp907481q
106. Boita, J.; Castegnaro, M. V.; Alves, M. D. M.; Morais, J. A dispenser-reactor apparatus applied for in situ XAS monitoring of Pt nanoparticle formation J. Synchrotron Radiat. 2015, 22, 736 10.1107/S1600577515003434
107. Hench, L. L.; West, J. K. The Sol-Gel Process Chem. Rev. 1990, 90, 33 10.1021/cr00099a003
108. Danks, A. E.; Hall, S. R.; Schnepp, Z. The evolution of 'sol-gel' chemistry as a technique for materials synthesis Mater. Horiz. 2016, 3, 91 10.1039/C5MH00260E
109. Olliges-Stadler, I.; Stotzel, J.; Koziej, D.; Rossell, M. D.; Grunwaldt, J. D.; Nachtegaal, M.; Frahm, R.; Niederberger, M. Study of the Chemical Mechanism Involved in the Formation of Tungstite in Benzyl Alcohol by the Advanced QEXAFS Technique Chem.-Eur. J. 2012, 18, 2305 10.1002/chem.201101514
110. Caetano, B. L.; Meneau, F.; Santilli, C. V.; Pulcinelli, S. H.; Magnani, M.; Briois, V. Mechanisms of SnO2 Nanoparticles Formation and Growth in Acid Ethanol Solution Derived from SAXS and Combined Raman-XAS Time-Resolved Studies Chem. Mater. 2014, 26, 6777 10.1021/cm5032688
111. Briois, V.; Belin, S.; Chalaca, M. Z.; Santos, R. H. A.; Santilli, C. V.; Pulcinelli, S. H. Solid-state and solution structural study of acetylacetone-modified tin(IV) chloride used as a precursor of SnO2 nanoparticles prepared by a sol-gel route Chem. Mater. 2004, 16, 3885 10.1021/cm040141q
112. McPeak, K. M.; Becker, M. A.; Britton, N. G.; Majidi, H.; Bunker, B. A.; Baxter, J. B. In Situ X-ray Absorption Near-Edge Structure Spectroscopy of ZnO Nanowire Growth During Chemical Bath Deposition Chem. Mater. 2010, 22, 6162 10.1021/cm102155m
113. Zhou, Y.; Grunwaldt, J. D.; Krumeich, F.; Zheng, K. B.; Chen, G. R.; Stotzel, J.; Frahm, R.; Patzke, G. R. Hydrothermal Synthesis of Bi6S2O15 Nanowires: Structural, in situ EXAFS, and Humidity-Sensing Studies Small 2010, 6, 1173 10.1002/smll.201000112
114. Chang, S. Y.; Uehara, A.; Booth, S. G.; Ignatyev, K.; Mosselmans, J. F. W.; Dryfe, R. A. W.; Schroeder, S. L. M. Structure and bonding in Au(I) chloride species: a critical examination of X-ray absorption spectroscopy (XAS) data RSC Adv. 2015, 5, 6912 10.1039/C4RA13087A
115. Yao, T.; Liu, S. J.; Sun, Z. H.; Li, Y. Y.; He, S.; Cheng, H.; Xie, Y.; Liu, Q. H.; Jiang, Y.; Wu, Z. Y.; Pan, Z. Y.; Yan, W. S.; Wei, S. Q. Probing Nucleation Pathways for Morphological Manipulation of Platinum Nanocrystals J. Am. Chem. Soc. 2012, 134, 9410 10.1021/ja302642x
116. Boita, J.; Nicolao, L.; Alves, M. C. M.; Morais, J. Observing Pt nanoparticle formation at the atomic level during polyol synthesis Phys. Chem. Chem. Phys. 2014, 16, 17640 10.1039/C4CP01925C
117. Harada, M.; Kamigaito, Y. Nucleation and Aggregative Growth Process of Platinum Nanoparticles Studied by in Situ Quick XAFS Spectroscopy Langmuir 2012, 28, 2415 10.1021/la204031j
118. Kranzlin, N.; van Beek, W.; Niederberger, M.; Koziej, D. Mechanistic Studies as a Tool for the Design of Copper-Based Heterostructures Adv. Mater. Interfaces 2015, 10.1002/admi.201500094
119. Jaumot, J.; de Juan, A.; Tauler, R. MCR-ALS GUI 2.0: New features and applications Chemom. Intell. Lab. Syst. 2015, 140, 1 10.1016/j.chemolab.2014.10.003
120. Hirsch, O.; Zeng, G. B.; Luo, L.; Staniuk, M.; Abdala, P. M.; van Beek, W.; Rechberger, F.; Suess, M. J.; Niederberger, M.; Koziej, D. Aliovalent Ni in MoO2 Lattice- Probing the Structure and Valence of Ni and Its Implication on the Electrochemical Performance Chem. Mater. 2014, 26, 4505 10.1021/cm501698a
121. Holmberg, V. C.; Helps, J. R.; Mkhoyan, K. A.; Norris, D. J. Imaging Impurities in Semiconductor Nanostructures Chem. Mater. 2013, 25, 1332 10.1021/cm400004x
122. Hiley, C. I.; Fisher, J. M.; Thompsett, D.; Kashtiban, R. J.; Sloan, J.; Walton, R. I. Incorporation of square-planar Pd2+ in fluorite CeO2: hydrothermal preparation, local structure, redox properties and stability J. Mater. Chem. A 2015, 3, 13072 10.1039/C5TA02007G
123. De Trizio, L.; Li, H. B.; Casu, A.; Genovese, A.; Sathya, A.; Messina, G. C.; Manna, L. Sn Cation Valency Dependence in Cation Exchange Reactions Involving Cu2-xSe Nanocrystals J. Am. Chem. Soc. 2014, 136, 16277 10.1021/ja508161c
124. Lesnyak, V.; George, C.; Genovese, A.; Prato, M.; Casu, A.; Ayyappan, S.; Scarpellini, A.; Manna, L. Alloyed Copper Chalcogenide Nanoplatelets via Partial Cation Exchange Reactions ACS Nano 2014, 8, 8407 10.1021/nn502906z
125. Jensen, K.; Christensen, M.; Tyrsted, C.; Iversen, B. B. Real-time synchrotron powder X-ray diffraction study of the antisite defect formation during sub- and supercritical synthesis of LiFePO4 and LiFe1-xMnx PO4 nanoparticles J. Appl. Crystallogr. 2011, 44, 287 10.1107/S0021889811006522
126. Oh, M. H.; Yu, T.; Yu, S. H.; Lim, B.; Ko, K. T.; Willinger, M. G.; Seo, D. H.; Kim, B. H.; Cho, M. G.; Park, J. H.; Kang, K.; Sung, Y. E.; Pinna, N.; Hyeon, T. Galvanic Replacement Reactions in Metal Oxide Nanocrystals Science 2013, 340, 964 10.1126/science.1234751
127. Yao, Y. L.; Patzig, C.; Hu, Y. F.; Scott, R. W. J. In Situ X-ray Absorption Spectroscopic Study of Fe@FexOy/Pd and Fe@FexOy/Cu Nanoparticle Catalysts Prepared by Galvanic Exchange Reactions J. Phys. Chem. C 2015, 119, 21209 10.1021/acs.jpcc.5b06155
128. Tyrsted, C.; Lock, N.; Jensen, K. M. O.; Christensen, M.; Bojesen, E. D.; Emerich, H.; Vaughan, G.; Billinge, S. J. L.; Iversen, B. B. Evolution of atomic structure during nanoparticle formation IUCrJ 2014, 1, 165 10.1107/S2052252514006538
129. Koziej, D.; Rossell, M. D.; Ludi, B.; Hintennach, A.; Novak, P.; Grunwaldt, J. D.; Niederberger, M. Interplay Between Size and Crystal Structure of Molybdenum Dioxide Nanoparticles-Synthesis, Growth Mechanism, and Electrochemical Performance Small 2011, 7, 377 10.1002/smll.201001606
130. Uehara, M.; Sun, Z. H.; Oyanagi, H.; Yamashita, K.; Fukano, A.; Nakamura, H.; Maeda, H. In situ extended x-ray absorption fine structure study of initial processes in CdSe nanocrystals formation using a microreactor Appl. Phys. Lett. 2009, 94, 063104 10.1063/1.3080660
131. Sun, Z. H.; Oyanagi, H.; Uehara, M.; Yamashita, K.; Fukano, A.; Maeda, H. In-situ EXAFS study of nucleation process of CdSe nanocrystals J. Phys. Conf. Ser. 2009, 190, 012120 10.1088/1742-6596/190/1/012120
132. Sun, Z. H.; Oyanagi, H.; Nakamura, H.; Jiang, Y.; Zhang, L.; Ullehara, M.; Yamashita, K.; Fukano, A.; Maeda, H. Ligand Effects of Amine on the Initial Nucleation and Growth Processes of CdSe Nanocrystals J. Phys. Chem. C 2010, 114, 10126 10.1021/jp101345n
133. Carino, E. V.; Kim, H. Y.; Henkelman, G.; Crooks, R. M. Site-Selective Cu Deposition on Pt Dendrimer-Encapsulated Nanoparticles: Correlation of Theory and Experiment J. Am. Chem. Soc. 2012, 134, 4153 10.1021/ja209115e
134. Chen, L. Y.; Chen, C. H.; Tseng, C. H.; Lai, F. L.; Hwang, B. J. Synthesis CdSexS1-x core/shell type quantum dots via one injection method Chem. Commun. 2011, 47, 1592 10.1039/C0CC04074F
135. Newton, M. A.; Belver-Coldeira, C.; Martinez-Arias, A.; Fernandez-Garcia, M. Dynamic in situ observation of rapid size and shape change of supported Pd nanoparticles during CO/NO cycling Nat. Mater. 2007, 6, 528 10.1038/nmat1924
136. Nashner, M. S.; Frenkel, A. I.; Somerville, D.; Hills, C. W.; Shapley, J. R.; Nuzzo, R. G. Core shell inversion during nucleation and growth of bimetallic Pt/Ru nanoparticles J. Am. Chem. Soc. 1998, 120, 8093 10.1021/ja980638z
137. Sagan, C. Wonder and Skepticism. Skeptical Inquirer 1995, 19 (January/February).