Limits of coherent x ray diffraction for imaging small crystals
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Limits of Coherent X-ray Diffraction for Imaging Small Crystals. Ian Robinson Ivan Vartanyants Franz Pfeiffer Mark Pfeifer Garth Williams. Department of Physics University of Illinois Second International Workshop on Noncrystallographic Phase Retrieval. Outline. Nanocrystal Shapes

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Limits of Coherent X-ray Diffraction for Imaging Small Crystals

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Limits of coherent x ray diffraction for imaging small crystals

Limits of Coherent X-ray Diffraction for Imaging Small Crystals

  • Ian Robinson

  • Ivan Vartanyants

  • Franz Pfeiffer

  • Mark Pfeifer

  • Garth Williams

Department of Physics

University of Illinois

Second International Workshop on

Noncrystallographic Phase Retrieval

I. K. Robinson, Phasing Workshop, June 2003


Outline

Outline

  • Nanocrystal Shapes

  • Vortices During Phasing

  • How small can we go?

  • Future Directions of CXD

I. K. Robinson, Phasing Workshop, June 2003


Lensless x ray microscope

Lensless X-ray Microscope

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

SEMS

  • Au blanket film

  • Quartz substrate

  • Annealed at 950°C for 70 hrs.

I. K. Robinson, Phasing Workshop, June 2003


Micron sized gold crystal 111 bragg reflection

Micron-sized gold crystal:(111) Bragg reflection

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

Imaging of Lattice Strains

I. K. Robinson, Phasing Workshop, June 2003


Symmetrized data and two best fits chisq 0 0005

Symmetrized Data and two best fitsChisq=0.0005

I. K. Robinson, Phasing Workshop, June 2003


2d reconstructions chisquare 0 0005

2D Reconstructionschisquare = 0.0005

I. K. Robinson, Phasing Workshop, June 2003


3d diffraction method

3D Diffraction Method

kf

Q=kf - ki

ki

I. K. Robinson, Phasing Workshop, June 2003


3d diffraction data 1 micron au crystal

3D Diffraction Data1 micron Au crystal

* Center is Symmetric *

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

111

111

Slices through plan view SEM:

I. K. Robinson, Phasing Workshop, June 2003


Generic error reduction method

Generic “Error Reduction” method

J. R. Fienup Appl. Opt. 21 2758 (1982)

R. W. Gerchberg and W. O. Saxton Optik 35 237 (1972)

I. K. Robinson, Phasing Workshop, June 2003


Real space constraints in crystallograhy r p millane j opt soc am a 13 725 1996

Real-space Constraints in CrystallograhyR. P. Millane, J. Opt. Soc Am. A 13 725 (1996)

  • ‘Positivity’ constraint (Sayre)

  • Finite support, molecular envelope

  • Solvent flattening

  • Molecular replacement

  • Non-crystallographic symmetry

  • Non-uniqueness is ‘pathologically rare’ (d>1)

I. K. Robinson, Phasing Workshop, June 2003


Phasing using g s algorithm

cut off “support”

Phasing using G-S Algorithm

I. K. Robinson, Phasing Workshop, June 2003


Convergence trajectory

Convergence Trajectory

wide support

narrow support

I. K. Robinson, Phasing Workshop, June 2003


Alternation of er and hio helps to avoid stagnation

Alternation of ER and HIOHelps to avoid stagnation

I. K. Robinson, Phasing Workshop, June 2003


Incomplete reconstruction can be striped 0 5 micron pb crystal on sio 2 substrate

Incomplete Reconstruction can be Striped0.5 micron Pb crystal on SiO2 substrate

I. K. Robinson, Phasing Workshop, June 2003


Stripes caused by vortices vortex pairs separated by inverse of stripe spacing

Stripes caused by “Vortices”Vortex pairs separated by inverse of stripe spacing

I. K. Robinson, Phasing Workshop, June 2003


Result of patching in 2d

Result of “Patching” in 2D

I. K. Robinson, Phasing Workshop, June 2003


3d vortices form pairs of loops

3D Vortices Form Pairs of Loops

I. K. Robinson, Phasing Workshop, June 2003


Vortices are a cause of stagnation during error reduction

Vortices are a Cause of Stagnation during Error Reduction

Lauren Perskie, UIUC Summer student

Number of vortices / 104

Chisquare

I. K. Robinson, Phasing Workshop, June 2003


Cxd beamline at aps sector 34

CXD Beamline at APS Sector 34

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

I. K. Robinson, Phasing Workshop, June 2003


Roller blade slits in uhv

Roller-Blade Slits in UHV

I. K. Robinson, Phasing Workshop, June 2003


Lensless x ray microscope1

Lensless X-ray Microscope

I. K. Robinson, Phasing Workshop, June 2003


Cxd from silver nanocubes

CXD from Silver Nanocubes

Yugang Sun and Younan Xia, Science 298 2177 (2003)

I. K. Robinson, Phasing Workshop, June 2003


170nm silver nanocubes

170nm Silver Nanocubes

I. K. Robinson, Phasing Workshop, June 2003


Structure in yoneda peak grazing exit diffraction from a 1000a au polycrystalline film

Structure in “Yoneda” PeakGrazing-exit diffraction from a 1000A Au polycrystalline film

Specular (αf ~ αi)

αf ~ αc

αf ~ 0


Competitive grain growth c v thompson ann rev mat sci 30 159 2000

Competitive Grain GrowthC. V. Thompson, Ann. Rev. Mat. Sci. 30 159 (2000)

αf~αc

αf<αc

I. K. Robinson, Phasing Workshop, June 2003


Angle series 0 01 steps

Angle series, 0.01° steps

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

Low dislocationdensity GeSi filmsThickness close to critical thicknessDislocations aggregate at interface and glide to surface along {111}T. Spila, UIUC Thesis

I. K. Robinson, Phasing Workshop, June 2003


Limits of coherent x ray diffraction for imaging small crystals

I. K. Robinson, Phasing Workshop, June 2003


Ge x si 1 x film diffraction

GexSi1-x Film Diffraction

  • 202 Bragg Peak

  • 2800A film

  • 2° incidence angle

  • 8.5 keV

  • 20μm ×40μm beam

  • onto KB mirror

  • 1μm ×1μm focus

  • 0.5μm sample steps

  • APS 34-ID-C

I. K. Robinson, Phasing Workshop, June 2003


Conclusions and outlook

Conclusions and Outlook

  • Inversion of CXD by ER-HIO methods

  • Internal structure of Au Nanocrystals

  • Preservation of coherence upon focussing

  • Smallest size now down to 170nm

  • New CXD-Yoneda geometry

  • Dislocation strain structure may be possible

I. K. Robinson, Phasing Workshop, June 2003


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