Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain; however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ∼280°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.

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Micro-beam Laue alignment of multi-reflection Bragg coherent diffraction imaging measurements

Journal of Synchrotron Radiation ◽

10.1107/s1600577517009183 ◽

2017 ◽

Vol 24 (5) ◽

pp. 1048-1055 ◽

Cited By ~ 13

Author(s):

Felix Hofmann ◽

Nicholas W. Phillips ◽

Ross J. Harder ◽

Wenjun Liu ◽

Jesse N. Clark ◽

...

Keyword(s):

Focused Ion Beam ◽

Lattice Strain ◽

Ion Beam ◽

Strain Tensor ◽

Three Dimensional ◽

Stress Fields ◽

X Ray Diffraction ◽

X Ray ◽

Coherent Diffraction Imaging ◽

Diffraction Imaging

Multi-reflection Bragg coherent diffraction imaging has the potential to allow three-dimensional (3D) resolved measurements of the full lattice strain tensor in specific micro-crystals. Until now such measurements were hampered by the need for laborious, time-intensive alignment procedures. Here a different approach is demonstrated, using micro-beam Laue X-ray diffraction to first determine the lattice orientation of the micro-crystal. This information is then used to rapidly align coherent diffraction measurements of three or more reflections from the crystal. Based on these, 3D strain and stress fields in the crystal are successfully determined. This approach is demonstrated on a focused ion beam milled micro-crystal from which six reflections could be measured. Since information from more than three independent reflections is available, the reliability of the phases retrieved from the coherent diffraction data can be assessed. Our results show that rapid, reliable 3D coherent diffraction measurements of the full lattice strain tensor in specific micro-crystals are now feasible and can be successfully carried out even in heavily distorted samples.

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ON THE MEASUREMENT AND INTERPRETATION OF RESIDUAL STRESS AT THE MICRO-SCALE

International Journal of Modern Physics B ◽

10.1142/s0217979210063910 ◽

2010 ◽

Vol 24 (01n02) ◽

pp. 1-9 ◽

Cited By ~ 3

Author(s):

ALEXANDER M. KORSUNSKY ◽

EDOARDO BEMPORAD ◽

MARCO SEBASTIANI ◽

FELIX HOFMANN ◽

SARAANSH DAVE

Keyword(s):

Residual Stress ◽

Focused Ion Beam ◽

Ion Beam ◽

X Ray Diffraction ◽

Strain Relief ◽

X Ray ◽

Micro Scale ◽

Digital Correlation ◽

Non Destructive

In the present paper we consider two representative methods for residual stress evaluation at the micro-scale: a (semi-)destructive method involving material removal and the measurement of strain relief; and a non-destructive X-ray diffraction technique involving the use of micro-focused synchrotron X-ray beam. A recently developed strain relief approach is described using a Focused Ion Beam (FIB) to create a circular trench of progressively increasing depth around a circular "island". Residual stress is evaluated by the comparison of the strain relief (measured by digital correlation of displacements or strains) with Finite Element simulations. The technique is illustrated for a thin TiN coating layer. The second approach uses focused synchrotron X-ray beams for white beam Laue diffraction. Demonstration experiments described involve in situ loading of commercially pure nickel foil. Procedures for validation and improvement of accuracy are discussed.

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Dynamic observation of dislocation evolution and interaction with twin boundaries in silicon crystal growth using in – situ synchrotron X-ray diffraction imaging

Acta Materialia ◽

10.1016/j.actamat.2021.116819 ◽

2021 ◽

Vol 210 ◽

pp. 116819

Author(s):

M.G. Tsoutsouva ◽

G. Regula ◽

B. Ryningen ◽

P.E. Vullum ◽

N. Mangelinck-Noël ◽

...

Keyword(s):

Crystal Growth ◽

Silicon Crystal ◽

X Ray Diffraction ◽

Twin Boundaries ◽

X Ray ◽

Dynamic Observation ◽

Diffraction Imaging

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Oxidation of Alloy-X in Subcritical, Transition, and Supercritical Water

CORROSION ◽

10.5006/3881 ◽

2021 ◽

Author(s):

Zachary Karmiol ◽

Dev Chidambaram

Keyword(s):

Supercritical Water ◽

Photoelectron Spectroscopy ◽

Focused Ion Beam ◽

Elevated Temperatures ◽

Subcritical Water ◽

Ion Beam ◽

X Ray Diffraction ◽

X Ray ◽

Nickel Based Superalloy ◽

Before And After

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

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Fiducial marker application method for position alignment of in situ multimodal X-ray experiments and reconstructions

Journal of Applied Crystallography ◽

10.1107/s1600576716001989 ◽

2016 ◽

Vol 49 (2) ◽

pp. 700-704 ◽

Cited By ~ 12

Author(s):

Paul A. Shade ◽

David B. Menasche ◽

Joel V. Bernier ◽

Peter Kenesei ◽

Jun-Sang Park ◽

...

Keyword(s):

Focused Ion Beam ◽

Ion Beam ◽

Tensile Specimen ◽

Material Behavior ◽

Validation Data ◽

Great Opportunity ◽

Characterization Methods ◽

X Ray ◽

Multiple Data Sets

An evolving suite of X-ray characterization methods are presently available to the materials community, providing a great opportunity to gain new insight into material behavior and provide critical validation data for materials models. Two critical and related issues are sample repositioning during an in situ experiment and registration of multiple data sets after the experiment. To address these issues, a method is described which utilizes a focused ion-beam scanning electron microscope equipped with a micromanipulator to apply gold fiducial markers to samples for X-ray measurements. The method is demonstrated with a synchrotron X-ray experiment involving in situ loading of a titanium alloy tensile specimen.

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Growth of MBE-Codeposited IrSi3 on Si(111) and Si(100)

MRS Proceedings ◽

10.1557/proc-299-303 ◽

1994 ◽

Vol 299 ◽

Author(s):

Gary A. Gibson ◽

Davis A. Lange ◽

Charles M. Falco

Keyword(s):

Ion Beam ◽

Silicide Phase ◽

X Ray Diffraction ◽

X Ray ◽

Low Energy Electron Diffraction ◽

Growth Modes ◽

Transmission Electron ◽

Low Energy Electron

AbstractWe have used Molecular Beam Epitaxy (MBE) to successfully grow films that are predominantly IrSi3 on both Si(111) and Si(100) substrates by codeposition of Si and Ir in a 3:1 ratio. Bragg-Brentano and Seemann-Bohlin x-ray diffraction reveal that polycrystalline IrSi3 films form as low as 450 °C. This is the lowest temperature yet reported for growth of this iridium silicide phase. These x-ray diffraction techniques, along with Transmission Electron Microscope (TEM) diffraction and in situ Low Energy Electron Diffraction (LEED), show that at higher deposition temperatures codeposition can form IrSi3 films on Si(111) that consist predominantly of a single epitaxial growth orientation. Ion beam channeling and x-ray rocking curves show that the epitaxial quality of IrSi3 films deposited on Si(111) is superior to that of IrSi3 films deposited on Si(100). We also present evidence for several new epitaxial IrSi3 growth modes on Si(111) and Si(100).

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Structural Characterization of Ion Beam Enhanced Solid Phase Epitaxial Regrowth by Raman, RBS, and X-Ray Analysis

MRS Proceedings ◽

10.1557/proc-126-177 ◽

1988 ◽

Vol 126 ◽

Author(s):

John F. Knudsen ◽

R. C. Bowman ◽

P. M. Adams ◽

R. Newman ◽

J. P. Hurrell ◽

...

Keyword(s):

Solid Phase ◽

Ion Beam ◽

Beam Current ◽

Crystalline Quality ◽

X Ray Diffraction ◽

X Ray ◽

Epitaxial Regrowth ◽

High Beam Current

ABSTRACTEpitaxial regrowth of deposited amorphous silicon has been previously described utilizing ion implantation amorphization, ion mixing and thermal anneal. This paper evaluates the effects of these process steps on crystalline quality utilizing Rutherford Backscattering (RBS), x-ray diffraction rocking curves and Raman scattering.In situ (during implantation) regrowth results in defective crystallinity. In contrast, when there is no in situ regrowth, the post anneal crystallinity is equivalent by RBS and x-ray evaluation to virgin single crystal wafers. In situ regrowth is most pronounced during the high beam current ion mixing type implants which produce wafer temperatures of about 250°C. The final crystalline quality which results from different sequences of amorphization and ion mixing implants, is strongly dependent upon the amount of in situ regrowth which has occurred. The greater the in situ regrowth the poorer the final crystalline quality.

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Toward in situ x-ray diffraction imaging at the nanometer scale

10.1117/12.794438 ◽

2008 ◽

Cited By ~ 2

Author(s):

Nadia A. Zatsepin ◽

Ruben A. Dilanian ◽

Andrei Y. Nikulin ◽

Brian M. Gable ◽

Barry C. Muddle ◽

...

Keyword(s):

Nanometer Scale ◽

X Ray Diffraction ◽

X Ray ◽

Diffraction Imaging

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Dislocation sources and slip band nucleation from indents on silicon wafers

Journal of Applied Crystallography ◽

10.1107/s0021889810029894 ◽

2010 ◽

Vol 43 (5) ◽

pp. 1036-1039 ◽

Cited By ~ 12

Author(s):

J. Wittge ◽

A. N. Danilewsky ◽

D. Allen ◽

P. McNally ◽

Z. Li ◽

...

Keyword(s):

Thermal Annealing ◽

Slip Band ◽

Rapid Thermal Annealing ◽

Line Tension ◽

X Ray Diffraction ◽

X Ray ◽

Diffraction Imaging ◽

Dislocation Sources ◽

Nucleation Of Dislocations

The nucleation of dislocations at controlled indents in silicon during rapid thermal annealing has been studied byin situX-ray diffraction imaging (topography). Concentric loops extending over pairs of inclined {111} planes were formed, the velocities of the inclined and parallel segments being almost equal. Following loss of the screw segment from the wafer, the velocity of the inclined segments almost doubled, owing to removal of the line tension of the screw segments. The loops acted as obstacles to slip band propagation.

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