PMID- 37639375 OWN - NLM STAT- Publisher LR - 20230929 IS - 1435-8115 (Electronic) IS - 1431-9276 (Linking) VI - 29 IP - 5 DP - 2023 Sep 29 TI - Using Focused Ion Beam Time-of-Flight Secondary Ion Mass Spectrometry to Depth Profile Nanoparticles in Polymer Nanocomposites. PG - 1557-1565 LID - 10.1093/micmic/ozad085 [doi] AB - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a versatile surface-sensitive technique for characterizing both hard and soft matter. Its chemical and molecular specificity, high spatial resolution, and superior sensitivity make it an ideal method for depth profiling polymeric systems, including those comprised of both inorganic and organic constituents (i.e., polymer nanocomposites, PNCs). To best utilize ToF-SIMS for characterizing PNCs, experimental conditions must be optimized to minimize challenges such as the matrix effect and charge accumulation. Toward that end, we have successfully used ToF-SIMS with a Xe+ focused ion beam to depth profile silica nanoparticles grafted with poly(methyl methacrylate) (PMMA-NP) in a poly(styrene-ran-acrylonitrile) matrix film by selecting conditions that address charge compensation and the primary incident beam angles. By tracking the sputtered Si+ species and fitting the resultant concentration profile, the diffusion coefficient of PMMA-NP was determined to be D = 2.4 x 10-14 cm2/s. This value of D lies between that measured using Rutherford backscattering spectrometry (6.4 x 10-14 cm2/s) and the value predicted by the Stokes-Einstein model (2.5 x 10-15 cm2/s). With carefully tuned experimental parameters, ToF-SIMS holds great potential for quantitatively characterizing the nanoparticles at the surfaces and interfaces within PNC materials as well as soft matter in general. CI - (c) The Author(s) 2023. Published by Oxford University Press on behalf of the Microscopy Society of America. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com. FAU - Zhang, Aria C AU - Zhang AC AUID- ORCID: 0000-0002-7927-7912 AD - Materials Science and Engineering, University of Pennsylvania, 3231 Walnut Street, Philadelphia, Pennsylvania 19104, USA. AD - Materials Research Science & Engineering Center (MRSEC), University of Pennsylvania, 3231 Walnut Street, Philadelphia 19104, USA. FAU - Maguire, Shawn M AU - Maguire SM AUID- ORCID: 0000-0002-5317-4990 AD - Materials Science and Engineering, University of Pennsylvania, 3231 Walnut Street, Philadelphia, Pennsylvania 19104, USA. FAU - Ford, Jamie T AU - Ford JT AUID- ORCID: 0000-0002-7657-2465 AD - Nanoscale Characterization Facility, University of Pennsylvania, 3205 Walnut Street, Philadelphia, Pennsylvania 19104, USA. FAU - Composto, Russell J AU - Composto RJ AD - Materials Science and Engineering, University of Pennsylvania, 3231 Walnut Street, Philadelphia, Pennsylvania 19104, USA. AD - Materials Research Science & Engineering Center (MRSEC), University of Pennsylvania, 3231 Walnut Street, Philadelphia 19104, USA. LA - eng GR - NSF/ GR - DMR1905912/DMR Polymers Program/ GR - MRSEC-DMR-1720530/University of Pennsylvania/ PT - Journal Article PL - England TA - Microsc Microanal JT - Microscopy and microanalysis : the official journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada JID - 9712707 SB - IM OTO - NOTNLM OT - depth profiles OT - diffusion OT - polymer nanocomposites OT - surface and interface OT - time-of-flight secondary ion mass spectrometry COIS- Conflict of Interest The authors declare that they have no competing interest. EDAT- 2023/08/28 18:41 MHDA- 2023/08/28 18:41 CRDT- 2023/08/28 13:12 PHST- 2023/05/02 00:00 [received] PHST- 2023/07/10 00:00 [revised] PHST- 2023/07/30 00:00 [accepted] PHST- 2023/08/28 18:41 [pubmed] PHST- 2023/08/28 18:41 [medline] PHST- 2023/08/28 13:12 [entrez] AID - 7252807 [pii] AID - 10.1093/micmic/ozad085 [doi] PST - ppublish SO - Microsc Microanal. 2023 Sep 29;29(5):1557-1565. doi: 10.1093/micmic/ozad085.