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Title: 3D lattice distortions and defect structures in ion-implanted nano-crystals

Abstract

The ability of Focused Ion Beam (FIB) techniques to cut solid matter at the nano-scale revolutionized the study of material structure across the life-, earth- and material sciences. But a detailed understanding of the damage caused by the ion beam and its effect on material properties remains elusive. We examine this damage in 3D using coherent X-ray diffraction to measure the full lattice strain tensor in FIB-milled gold nano-crystals. We also found that even very low ion doses, previously thought to be negligible, cause substantial lattice distortions. At higher doses, extended self-organized defect structures appear. Combined with detailed numerical calculations, these observations allow fundamental insight into the nature of the damage created and the structural instabilities that lead to a surprisingly inhomogeneous morphology.

Authors:
 [1];  [2];  [3];  [4];  [5];  [5];  [6];  [7];  [4];  [3]
  1. Univ. of Oxford (United Kingdom). Dept. of Engineering Science
  2. Univ. College, London (United Kingdom). London Centre for Nanotechnology; Science and Technology Facilities Council (STFC), Oxford (United Kingdom). Rutherford Appleton Lab. (RAL)
  3. Univ. of Oxford (United Kingdom). Dept. of Materials
  4. Argonne National Lab. (ANL), Argonne, IL (United States). Advanced Photon Source
  5. La Trobe Univ., Melbourne, VIC (Australia). ARC Centre of Advanced Molecular Imaging; CSIRO Manufacturing Flagship, CAN Parkville (Australia)
  6. SLAC National Accelerator Lab., Menlo Park, CA (United States); Deutsches Elektronen-Synchrotron (DESY), Hamburg (Germany). Center for Free-Electron Laser Science
  7. La Trobe Univ., Melbourne, VIC (Australia). ARC Centre of Advanced Molecular Imaging
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL), Upton, NY (United States); SLAC National Accelerator Lab., Menlo Park, CA (United States); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1349558
Alternate Identifier(s):
OSTI ID: 1360215; OSTI ID: 1390607
Report Number(s):
BNL-113662-2017-JA
Journal ID: ISSN 2045-2322; R&D Project: PO011; KC0201060
Grant/Contract Number:
SC00112704; AC02-76SF00515; AC02-06CH11357
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Scientific Reports
Additional Journal Information:
Journal Volume: 7; Journal ID: ISSN 2045-2322
Publisher:
Nature Publishing Group
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY

Citation Formats

Hofmann, Felix, Robinson, Ian K., Tarleton, Edmund, Harder, Ross J., Phillips, Nicholas W., Ma, Pui -Wai, Clark, Jesse N., Abbey, Brian, Liu, Wenjun, and Beck, Christian E. 3D lattice distortions and defect structures in ion-implanted nano-crystals. United States: N. p., 2017. Web. doi:10.1038/srep45993.
Hofmann, Felix, Robinson, Ian K., Tarleton, Edmund, Harder, Ross J., Phillips, Nicholas W., Ma, Pui -Wai, Clark, Jesse N., Abbey, Brian, Liu, Wenjun, & Beck, Christian E. 3D lattice distortions and defect structures in ion-implanted nano-crystals. United States. doi:10.1038/srep45993.
Hofmann, Felix, Robinson, Ian K., Tarleton, Edmund, Harder, Ross J., Phillips, Nicholas W., Ma, Pui -Wai, Clark, Jesse N., Abbey, Brian, Liu, Wenjun, and Beck, Christian E. Thu . "3D lattice distortions and defect structures in ion-implanted nano-crystals". United States. doi:10.1038/srep45993. https://www.osti.gov/servlets/purl/1349558.
@article{osti_1349558,
title = {3D lattice distortions and defect structures in ion-implanted nano-crystals},
author = {Hofmann, Felix and Robinson, Ian K. and Tarleton, Edmund and Harder, Ross J. and Phillips, Nicholas W. and Ma, Pui -Wai and Clark, Jesse N. and Abbey, Brian and Liu, Wenjun and Beck, Christian E.},
abstractNote = {The ability of Focused Ion Beam (FIB) techniques to cut solid matter at the nano-scale revolutionized the study of material structure across the life-, earth- and material sciences. But a detailed understanding of the damage caused by the ion beam and its effect on material properties remains elusive. We examine this damage in 3D using coherent X-ray diffraction to measure the full lattice strain tensor in FIB-milled gold nano-crystals. We also found that even very low ion doses, previously thought to be negligible, cause substantial lattice distortions. At higher doses, extended self-organized defect structures appear. Combined with detailed numerical calculations, these observations allow fundamental insight into the nature of the damage created and the structural instabilities that lead to a surprisingly inhomogeneous morphology.},
doi = {10.1038/srep45993},
journal = {Scientific Reports},
number = ,
volume = 7,
place = {United States},
year = {Thu Apr 06 00:00:00 EDT 2017},
month = {Thu Apr 06 00:00:00 EDT 2017}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record

Citation Metrics:
Cited by: 12works
Citation information provided by
Web of Science

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  • Focussed Ion Beam (FIB) milling is a mainstay of nano-scale machining. By manipulating a tightly focussed beam of energetic ions, often gallium (Ga+), FIB can sculpt nanostructures via localised sputtering. This ability to cut solid matter on the nano-scale revolutionised sample preparation across the life, earth and materials sciences. Despite its widespread usage, detailed understanding of the FIBinduced structural damage, intrinsic to the technique, remains elusive. Here we examine the defects caused by FIB in initially pristine objects. Using Bragg Coherent X-ray Diffraction Imaging (BCDI), we are able to spatially-resolve the full lattice strain tensor in FIB-milled gold nano-crystals. Wemore » find that every use of FIB causes large lattice distortions. Even very low ion doses, typical of FIB imaging and previously thought negligible, have a dramatic effect. Our results are consistent with a damage microstructure dominated by vacancies, highlighting the importance of free-surfaces in determining which defects are retained. At larger ion fluences, used during FIB-milling, we observe an extended dislocation network that causes stresses far beyond the bulk tensile strength of gold. These observations provide new fundamental insight into the nature of the damage created and the defects that lead to a surprisingly inhomogeneous morphology.« less
  • Here, this study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strainsmore » have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of Burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.« less