Extension of Rietveld Refinement for Benchtop Powder XRD Analysis of Ultrasmall Supported Nanoparticles
Source abstract
Abstract
We present a method for characterizing ultrasmall (<2 nm) supported crystallites with benchtop XRD. Central to the method is an understanding of the intensity effects at play; these intensity effects and their corrections are discussed in depth. Background subtraction─long considered one of the main barriers to ultrasmall crystal characterization─is solved by correcting the diffractogram of a separately measured support for the relevant intensity effects. Rietveld refinement is demonstrated to be an adequate analysis method for the general characterization of simple nanosystems. A 4.8% Pt/SiO2 sample (1.3 nm, volume-weighted average) is used as a case study; it is found that the Pt spontaneously oxidizes under ambient conditions and consists of a metallic core surrounded by a PtO2 shell. Both phases have average dimensions smaller than 1 nm. The XRD results also suggest lattice expansion of the Pt core as compared to bulk Pt.
Source: openalex_inverted_index · Quality: baseline
Research context
OpenAlex topics: X-ray Diffraction in Crystallography · X-ray Spectroscopy and Fluorescence Analysis · Machine Learning in Materials Science
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
University of South Carolina, Columbia, South Carolina 29201, United States
SLAC National Accelerator Laboratory, Menlo Park, California 94025, United States
Department of Inorganic Chemistry, Fritz Haber Institute of the Max Planck Society, Berlin 14195, Germany
Funding
Division of Graduate Education · South Carolina Smart State Center of Catalysis for Renewable Fuels, University of South Carolina
References (54)
Show source-provided references
1. 10.1126/science.aao653810.1126/science.aao6538 ↗
2. 10.1016/j.jcat.2006.04.00410.1016/j.jcat.2006.04.004 ↗
3. 10.1039/C4CY00414K10.1039/C4CY00414K ↗
4. 10.1007/s10562-015-1479-610.1007/s10562-015-1479-6 ↗
5. 10.1016/S0926-860X(01)00892-410.1016/S0926-860X(01)00892-4 ↗
6. 10.1063/1.167426610.1063/1.1674266 ↗
7. 10.1107/S056773948100060010.1107/S0567739481000600 ↗
8. 10.1021/la00063a01310.1021/la00063a013 ↗
9. 10.1002/bbpc.1993097030310.1002/bbpc.19930970303 ↗
10. 10.1021/j100375a04310.1021/j100375a043 ↗
11. 10.1021/jp010065410.1021/jp0100654 ↗
12. 10.1021/jp803527z10.1021/jp803527z ↗
13. TOPAS, V.6.0; Bruker AXS, 2018.
14. Hubbel J. H. · 2004
15. 10.1017/S088571560001370110.1017/S0885715600013701 ↗
16. Zevin L. S. · 1995 · 10010.1007/978-1-4613-9535-5_4 ↗
17. 10.1080/1478644450852091810.1080/14786444508520918 ↗
18. Dinnebier R. E. · 2019
19. Pecharsky V. K. · 2009
20. 10.1017/S088571560001941210.1017/S0885715600019412 ↗
21. 10.1107/S010876738709924010.1107/S0108767387099240 ↗
22. 10.1107/S0365110X6400080910.1107/S0365110X64000809 ↗
23. 10.1107/S002188987200970710.1107/S0021889872009707 ↗
24. 10.1017/S088571560001787510.1017/S0885715600017875 ↗
25. 10.1107/S002188989800985610.1107/S0021889898009856 ↗
26. Lipp J. · 2022
27. 10.1016/j.jcat.2004.03.03410.1016/j.jcat.2004.03.034 ↗
28. 10.1016/j.jcat.2004.04.00710.1016/j.jcat.2004.04.007 ↗
29. 10.1111/jmi.1287710.1111/jmi.12877 ↗
30. 10.1107/S002188981003049910.1107/S0021889810030499 ↗
31. 10.1080/1478644330946219910.1080/14786443309462199 ↗
32. 10.1021/ja01850a07410.1021/ja01850a074 ↗
33. 10.1016/0022-5088(89)90148-310.1016/0022-5088(89)90148-3 ↗
34. 10.1016/0025-5408(87)90220-010.1016/0025-5408(87)90220-0 ↗
35. 10.1016/0022-5088(84)90338-210.1016/0022-5088(84)90338-2 ↗
36. Hoekstra H. R. · 1971 · 3910.1021/ba-1971-0098.ch004 ↗
37. 10.1021/ic501770g10.1021/ic501770g ↗
38. 10.1016/0022-5088(68)90070-210.1016/0022-5088(68)90070-2 ↗
39. 10.1063/1.175086010.1063/1.1750860 ↗
40. 10.1016/0022-1902(77)80270-410.1016/0022-1902(77)80270-4 ↗
41. 10.1016/0039-6028(89)90175-110.1016/0039-6028(89)90175-1 ↗
42. 10.1007/s10562-017-2060-210.1007/s10562-017-2060-2 ↗
43. 10.1103/PhysRevB.51.1096810.1103/PhysRevB.51.10968 ↗
44. 10.1080/0141861940824223910.1080/01418619408242239 ↗
45. 10.1016/0021-9517(87)90135-710.1016/0021-9517(87)90135-7 ↗
46. 10.1016/j.actamat.2009.09.06110.1016/j.actamat.2009.09.061 ↗
47. 10.1039/a904654b10.1039/a904654b ↗
48. 10.1039/C6CY00491A10.1039/C6CY00491A ↗
49. 10.1080/2055074X.2016.126317710.1080/2055074X.2016.1263177 ↗
50. 10.1021/jacs.8b0816210.1021/jacs.8b08162 ↗
51. Lipp, J. W. Fine Points for Broad Bumps: the Extension of Rietveld Refinement for Benchtop Powder XRD Analysis of Ultra-small Supported Nanoparticles, University of South Carolina, 2021.
52. 10.1002/ejic.20180053410.1002/ejic.201800534 ↗
53. 10.1021/acs.iecr.0c0125410.1021/acs.iecr.0c01254 ↗
54. Kaszkur Z. · 2015 · 147