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

We report on the results of a thorough in situ synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds in situ in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO3) and amount of the coordination modulator acetic acid (AcOH). When only HNO3 is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO3, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO3 slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO3 favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO3. Based on these in situ results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

Download Full-text

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

Journal of Synchrotron Radiation ◽

10.1107/s1600577520016264 ◽

2021 ◽

Vol 28 (2) ◽

pp. 550-565 ◽

Cited By ~ 1

Author(s):

David Yang ◽

Nicholas W. Phillips ◽

Kay Song ◽

Ross J. Harder ◽

Wonsuk Cha ◽

...

Keyword(s):

Focused Ion Beam ◽

Ion Beam ◽

Imaging Study ◽

X Ray Diffraction ◽

Multiple Reflections ◽

X Ray ◽

Self Diffusion ◽

Diffraction Imaging ◽

Gold Microcrystals

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.

Download Full-text

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

Download Full-text

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.

Download Full-text

Real‐time X‐ray diffraction imaging for semiconductor wafer metrology and high temperature in situ experiments

physica status solidi (a) ◽

10.1002/pssa.201184264 ◽

2011 ◽

Vol 208 (11) ◽

pp. 2499-2504 ◽

Cited By ~ 11

Author(s):

A. N. Danilewsky ◽

J. Wittge ◽

A. Hess ◽

A. Cröll ◽

A. Rack ◽

...

Keyword(s):

High Temperature ◽

Real Time ◽

X Ray Diffraction ◽

Semiconductor Wafer ◽

X Ray ◽

In Situ Experiments ◽

Diffraction Imaging

Download Full-text

Application of X-ray topography to USSR and Russian space materials science

IUCrJ ◽

10.1107/s2052252516003730 ◽

2016 ◽

Vol 3 (3) ◽

pp. 200-210 ◽

Cited By ~ 1

Author(s):

I. L. Shul'pina ◽

I. A. Prokhorov ◽

Yu. A. Serebryakov ◽

I. Zh. Bezbakh

Keyword(s):

Crystal Growth ◽

Materials Science ◽

Perfect Crystal ◽

Space Vehicles ◽

X Ray Diffraction ◽

Semiconductor Crystal ◽

X Ray ◽

Diffraction Imaging ◽

Crystallization Conditions ◽

Former Ussr

The authors' experience of the application of X-ray diffraction imaging in carrying out space technological experiments on semiconductor crystal growth for the former USSR and for Russia is reported, from the Apollo–Soyuz programme (1975) up to the present day. X-ray topography was applied to examine defects in crystals in order to obtain information on the crystallization conditions and also on their changes under the influence of factors of orbital flight in space vehicles. The data obtained have promoted a deeper understanding of the conditions and mechanisms of crystallization under both microgravity and terrestrial conditions, and have enabled the elaboration of terrestrial methods of highly perfect crystal growth. The use of X-ray topography in space materials science has enriched its methods in the field of digital image processing of growth striations and expanded its possibilities in investigating the inhomogeneity of crystals.

Download Full-text

Atmospheric coherent X-ray diffraction imaging for in situ structural analysis at SPring-8 Hyogo beamline BL24XU

Journal of Synchrotron Radiation ◽

10.1107/s1600577518006410 ◽

2018 ◽

Vol 25 (4) ◽

pp. 1229-1237

Author(s):

Yuki Takayama ◽

Yuki Takami ◽

Keizo Fukuda ◽

Takamasa Miyagawa ◽

Yasushi Kagoshima

Keyword(s):

Structural Analysis ◽

Control Device ◽

Photon Flux ◽

X Rays ◽

Atmospheric Conditions ◽

X Ray Diffraction ◽

Macroporous Silica ◽

X Ray ◽

Diffraction Imaging

Coherent X-ray diffraction imaging (CXDI) is a promising technique for non-destructive structural analysis of micrometre-sized non-crystalline samples at nanometre resolutions. This article describes an atmospheric CXDI system developed at SPring-8 Hyogo beamline BL24XU for in situ structural analysis and designed for experiments at a photon energy of 8 keV. This relatively high X-ray energy enables experiments to be conducted under ambient atmospheric conditions, which is advantageous for the visualization of samples in native states. The illumination condition with pinhole-slit optics is optimized according to wave propagation calculations based on the Fresnel–Kirchhoff diffraction formula so that the sample is irradiated by X-rays with a plane wavefront and high photon flux of ∼1 × 1010 photons/16 µmø(FWHM)/s. This work demonstrates the imaging performance of the atmospheric CXDI system by visualizing internal voids of sub-micrometre-sized colloidal gold particles at a resolution of 29.1 nm. A CXDI experiment with a single macroporous silica particle under controlled humidity was also performed by installing a home-made humidity control device in the system. The in situ observation of changes in diffraction patterns according to humidity variation and reconstruction of projected electron-density maps at 5.2% RH (relative humidity) and 82.6% RH at resolutions of 133 and 217 nm, respectively, were accomplished.

Download Full-text

Investigation by coherent X-ray section topography of ferroelectric domain behaviour as a function of temperature in periodically poled Rb:KTP

Journal of Applied Crystallography ◽

10.1107/s0021889811012532 ◽

2011 ◽

Vol 44 (3) ◽

pp. 462-466 ◽

Cited By ~ 8

Author(s):

Fabio Masiello ◽

Tamzin A. Lafford ◽

Petra Pernot ◽

José Baruchel ◽

Dean S. Keeble ◽

...

Keyword(s):

Curie Temperature ◽

Ferroelectric Domain ◽

Potassium Titanyl Phosphate ◽

X Ray Diffraction ◽

Periodically Poled ◽

X Ray ◽

Ferroelectric Domains ◽

Diffraction Imaging ◽

Section Topography

The behaviour of ferroelectric domains at high temperatures near the Curie temperature in a periodically poled rubidium-doped potassium titanyl phosphate crystal (Rb:KTP) has been studied by Bragg–Fresnel X-ray diffraction imagingin situusing a compact coherence-preserving furnace. The development and partial disappearance of the inverted domain structure as the temperature increases has been successfully modelled, and is explained by invoking a built-in electric field produced under heating in a low vacuum by out-diffusion of atoms from the sample.

Download Full-text