Tiqiao XiaoEmail: tqxiao@sinap.ac.cn

Shanghai Synchrotron Radiation Facility

Dynamic X-ray Imaging and its Applications

ULITIMA 2018 Sept. 10-15,2018, ANL, Chicago, USA

ULITIMA 2018

2

Contents

◼ Brief to X-ray Imaging Group@SSRF

◼ Two dimensional X-ray dynamic imaging

◼ Dynamic X-ray CT imaging

◼ New contrast mechanism for X-ray imaging

◼ Conclusions

SSRF Complex

<5nm-rad

5 nm-rad

yx

B

1

Brightness & Emittance

NSLS-II

TPS

MAX-IV

10-1

XFEL higher brightness, shorter pulse

Current SR sources—towards lower emittance and higher brightness

X-ray Imaging Group @SSRF

Members

➢ 12 Staff

➢ Graduate students

➢ Postdoctors

➢ Guest scientists

Research Fields

➢ X-ray imaging

methodology

➢ Related applications

Based on SR & Lab source

Optical Hutch

End-station

0 20m 29m 32m 33m 35m 40m

CCDUndulator slits DCM Sample chamber and in-situ devices

slits ms-shutter μs-shutter

Bending

Magnet

Collimator

MirrorDCM Focusing

Mirror

Secondary

Source

Condenser

Zone Plate

Detector

0 20.5m 24m 26m 39m 41m 42m

Three X-ray Imaging Beamlines

BL13W--X-ray Imaging with wiggler source

Fast X-ray imaging beamline-Undulator source

X-ray nano-CT beamline-Bending Magnet

In operation

Under construction

Time

resolution

up to 80ps

Spatial

resolution

up to 20nm

ms, sub micron

Multi-Contrast Mechanism at SSRF

Contrast Method Information

Absorption m-CTComponents and structure for high Z materials (static-dynamic, quantitative)

Phase PC m-CTComponents and structure for low Z materials (static-dynamic, quantitative)

Fluorescence XFCT Elements distribution

Diffraction-XRD XRD-CTCrystal grain: location, orientation and morphology

Scattering-SAXS SAXS-CTNano particle: location and morphology

Moving Contrast MCXI complex system imaging

2nd order Photon Correlation

XGI-RS & FT Ghost Imaging

Nanostructure-lensless, turbulence free

A robust method for high-precision quantitative

analysis to the complex micro-vasculatures

𝑯𝒊𝒈𝒉 − 𝒍𝒆𝒗𝒆𝒍 𝒗𝒂𝒔𝒄𝒖𝒍𝒂𝒓 𝒓𝒂𝒕𝒊𝒐 =𝒂𝒗𝒆𝒓𝒂𝒈𝒆 𝒍𝒆𝒗𝒆𝒍

𝒎𝒂𝒙 𝒍𝒆𝒗𝒆𝒍

Hai Tan et al，J. Synchrotron Rad. (2016). 23, 1216-1226

Hai Tan et al，Nuclear Science and Techniques，(2016), 27:125

，DOI 10.1007/s41365-016-0121-7

used to evaluate the level of liver fibrosis

calcium oxalate cluster crystals

number volume

Linlin Ye et al, Journal of Ginseng Research (2016), doi: 10.1016/j.jgr.2016.05.004.

•Planted ginseng

•American ginseng

•Korean ginseng

•Wild ginseng

calcium oxalate cluster crystals

Identification of ginseng root using

quantitative X-ray microtomography

Sample: heterogeneous Junger

Basin shale

Composition and Porosity for oil shale

Fig1: Optical microscope image: Locations

of S1 (D: 0.8mm) and S4’ (D: 3mm) .Fig 2: Reconstructed slices of S1 (a) and S4’ (b). (c) Histograms.

Table 1: Porosities and the volume fractions

of the minerals in S1, S4’.

SR-μCT and reconstructions➢The X-ray beam energy: 25keV & 35keV

➢The sample-detector distance: 12 cm

➢The pixel size: 0.65μm (S1); 3.25μm (S4’)

data-constrained modelling microstructure

characterisation

The fractal dimensions of

the largest pore cluster of

S1 and S4’ : 2.34 and 2.86 .

Fig 3: Compositional distributions (a, b, e, f) and pore structures (c, g) of S1 and S4’. (d, h)

The frequency and volume distribution for pore clusters.

S1

S4’

Y.D. Wang et al 2016 JINST 11 C04005

XRD-CT developed for crystal characterization in alloys

近场探测器

Beamstop

样品台

狭缝

A method is developed to reveal the unknown minor phase within bulk

polycrystalline metals. Y.M. Yang et al., Materials Characterization 124 (2017) 206–214

XRD-CT developed for 3-D imaging to

granular crystal distribution and orientation

635℃ 645℃ 655℃

Morphology and texture characterization of crystal grains in bulk alloys processed by two-stage reheating

SAXS CT for polylactide(PLA)

• Poly(lactic acid) or polylactic acid or polylactide (PLA) is a biodegradable and bioactive thermoplastic aliphatic polyester derived from renewable resources, such as corn starch (in the United States and Canada), cassava roots, chips or starch (mostly in Asia), or sugarcane (in the rest of the world).

13

Conventional methods for crystal characterization

SEM AFM

POM SAXS/WAXD for slice samples

Applicable for surface or sliced samples

How to deal with volume samples?

SAXS-CT@SSRF

Vacuum pipeline

Sample

Pinhole

K-B mirror

Three dimensional Hierarchical Crystalline Structure Evolution in Injection-Molded Polylactide

Tao Hu et al, Applied Optics 56, 8326 (2017)

No obvious change of crystals observed along the fluids

3D distribution of PLA30 shish-kebab crystal(60 layers)

Fig 1. Sketch of the FF-XFCT with pinhole collimator

Fig 2. Reconstructed FF-XFCT and

transmission CT slices of the phantom Fig 3. 3D Cd and I imaging obtained by FF-XFCT

◆ Combine a FF-XFCT system with subtracting imaging, 3D elemental

distributions can be retrieved.

◆ FF-XFCT is a sensitive, inexpensive and simple approach for effective

3D element imaging.

Biao Deng et al, Analyst, 2015, 140, 3521–3525

X-ray full-field fluorescence tomography

17

Contents

◼ Brief to X-ray Imaging Group@SSRF

◼ Two dimensional X-ray dynamic imaging

◼ Dynamic X-ray CT imaging

◼ New contrast mechanism for X-ray imaging

◼ Conclusions

Micro-CT with X-ray tube

18Static and low resolution

2

21

3

2

)μ(μR

SNRΦ out

−=

Flux density needed for X-ray imaging,

where

SNR: signal to noise ratio,

R: spatial resolution,

m1-m2: contrast

To do something different—dynamic imaging preferred

high flux density of SR makes it possible for dynamic

X-ray imaging with high resolution and SNR

Why dynamic imaging preferred with SR

The First Live

imaging-Grasshopper

@BL13W

Broadcasted at

CCTV1

Dentritical

crystal growing

process

Ion transportation

in Lithium Cell

Dynamic X-ray imaging

Solidification behavior of alloystime scale: ms; spatial resolution: sub micron

Dendritic crystal growing process

No Electic Current EC: 7A/cm2

EC induced nucleation

Growing speed variation with temperature and time

Dendritic crystal growing speed with time

Solidification behavior and electromagnetic

Regulation Mechanism of Alloys—WANG TM’s group

300 µm

Physical Review E, 2010, 81: 042601

Materials Letter, 2012, 89: 137

300 µm

Dynamic X-ray imaging

Blood vessel related diseasesIn-vivo Imaging for vasculatures in rats—ms

Spatial resolution: microns

Vasculopathy on hypertensive rats

Wang L, et al. Front Aging Neurosci. 2017

SD

SHR

SHR

SD

Vessels for hypertensive

rats become narrower with

the wall turning thicker

Butylphthalide can stimulate the expanding of vascular

Qin C, et al, JCBFM, 2017

Dynamic X-ray imaging

Mechanisms for fuel spraytime scale: ms-ns; spatial resolution: micron

Setup for

imaging

system

Experiments on fuel spray_by WU Zhijun’s group, TJU

+

-

+

-

X光

慢速斩光器

喷油器

定容弹

闪烁晶体

可见光

镜子

高速摄像机

显微镜头

Kapton

窗口

27

Objects:

• Needle valve

movement

• Near field

spray

➢Driving electric current for needle valve

• Rising current(A): 6-7; 7-8; 8-9;9-10;10-11

• Keeping current(A): 3-4, 5-6, 6-7, 7-8

➢Frame rate of the CCD camera：40000 fps

➢Exposure time：23.4µs

➢Image size (pixel)：1024*512

➢Pixel size：2.5𝜇𝑚/pixel

Parameters for the experiments

Movement of needle valve—dynamic images

Exprimental Results

Near field spray—Pressure on Spray Crushing

Exprimental Results

➢Driving electric current for needle valve

• Rising current(A): 6-7

• Keeping current(A): 3-4

• Spray pulse: 2ms

➢Pressure for spray(MPa): 1,5,10,15

➢Frame rate: 70000 fps(14.3ms per frame)

➢Exposure time：248ns, 159ns

➢Image size (pixel)：1024*512

➢Pixel size：2.5𝜇𝑚/pixel

Pressure：1MPa

Pressure：14MPa

Dynamic image with 159ns exposure time @spray pressures

Near field spray—Pressure on Spray Crushing

32

Contents

◼ Brief to X-ray Imaging Group@SSRF

◼ Two dimensional X-ray dynamic imaging

◼ Dynamic X-ray CT imaging

◼ New contrast mechanism for X-ray imaging

◼ Conclusions

Dynamic CT—monochromatic beam

Xia et al., Nat. Commun. 2015

Glass transition

Physics on particle fluids— seconds to minutes

3d

2d

Flip process

T1 event 2-2 flip & 2-3/3-2 flip

Cao et al., Nat. Commun. 2018

Prof. Yujie Wang’ group

Monochromatic CT vs white beam

• Disadvantages (VS white beam)

– Lower flux intensity

– longer exposure time

– lower CT time resolution

• Advantages (VS white beam)

– Quantitative (bandwidth ~0.02% with DCM)

– Lower doseSam

ple

High

Energy

Low

Energy

Incident X-ray

(white beam)

Exit X-ray

Absorbed by

sample: Dose

Dose

reduce

sharply

Limited to 2 frames/s

PI air bearing rotation stage

Resolution 0.00004°

Repeatability 0.00005 °

Maximum speed

360 °/sec.

Wobble ± 1.25 μrad

Hamamatsu ORCA detector

Pixels 2048 (H)×2048 (V)

Pixel size 6.5 μm×6.5 μm

Frame rate Up to 1000 fps

Hamamatsu

ORCA detector

PI air bearing

rotation stage

Gas regulator

Gas pipeline

Quantitative micro-CT from 3D to 4D

Data collection（computer）

Memory 48G

Hard disk Solid state HD raid0

Collection & Saving

Collected directly in memory and then transferred to HD

GPU Parallel processing

Introduced to deal with the

massive data (48Gb/75s)

2Hz dynamic micro-CT

based on monochromatic

X-ray beam developed

A powerful tool for quantitative

analysis to 3D structure evolution

Anisotropic shrinkage of the insect’s air sacs

revealed in vivo by X-ray dynamic microtomography

2ms/projection, 136

projections, 500ms for

one set, lasting for 75s

with 150 breathing

points recorded

Liang Xu et. al., Scientific Reports, (2016), 6:32380 | DOI: 10.1038/srep32380

By Group of Prof. Xiaofang Hu from USTC

4D characterization of material microstructures

Microwave sintering of ceramics

Xu F et al. Applied Physics Letters, 2017, 110(10)

Quantification for drug release in operando

view from one project

ZHANG Jiweng’s Group@ SIMM

SSRF user’s results: Prof. Jiwen Zhang group @ SIMM

droplet releasing rate

Released droplet volume distribution

Dynamic CT—white beam

…catch faster process

Hardware of white beam dynamic CT

Shutter Filter Stages

Detector

Detector with higher efficiency

In house developed optics couple

system with camera installed

White beam optics coupling system

Commercial productIn house

developed

Magnification 2 5 7.5 10 8

NA 0.05 0.05 0.21 0.28 0.59

Working

distance (mm) 34 34 35 33.5 37

Coupling

efficiency (%) 0.11 0.17 3.4 6.5 27.5

⚫ In house developed L-shaped lens-coupled optical

microscopy system, it has larger NA and its coupling

efficiency is 8 times of existing commercial product.

⚫ Photron FASTCAM-SA-Z camera is installed in this

system, its pixel size is 20 μm with 1024×1024 pixels,

and a memory of 64GB. A maximum acquisition rate of

100000 fps under 640 ×280 pixels.

⚫ The actual pixel size of the detector system is 2.5μm,

FOV is 2.56mm × 2.56mm

FASTCAM-

SA-Z camera

Adjusting

system

Optics len

Scintillator

Experiment results

Live ant, 25Hz CTPlant root static sample, 26.6Hz CT

45

Contents

◼ Brief to X-ray Imaging Group@SSRF

◼ Two dimensional X-ray dynamic imaging

◼ Dynamic X-ray CT imaging

◼ New contrast mechanism for X-ray imaging

◼ Conclusions

New contrast mechanisms

• Moving Contrast X-ray imaging

• 2nd order X-ray photon correlation

46

Moving contrast X-ray imaging

◆ Imaging to complex system like a live body: all things are

moving and overlaping together. Is it possible to remove

these interference?

◆Concept of moving contrast: differentiate them by their

moving characteristics

Blood vessel imaging in vivo is critical to clinical diagnosis of many kinds of diseases

Tumor

Stroke

hypertension

Traditional solution: digital subtraction (DSA)

A mask image without contrast agent subtracted

from the angiogram—DSA, currently the

dominant clinic angiographic method

However, the human or rats are alive, it is hard to

hold tissues motionless inside the body—mask

different from the sequenced images for the

angiography →fake image and noises →solution?

Blood vessels Moving contrast image for other tissues

Static background − Mask imageHigh frequency noises

Results for moving contrast angiography

Interference of other tissues removed

and sensitivity of angiography greatly

improved by MCA

Water refilling process in leaf

Y.L. Xue, et al, Nucl Sci Tech, 24 60101-060101

Trace reconstructed by moving contrast X-ray imaging

53

2nd order Photon Correlation Imagingreal space ghost X-ray ghost imaging

Concept for 2nd order photon correlation X-ray imaging

Through the correlation between the reference and object

field, the information that is hidden inside the photon

fluctuations and abandoned by the traditional imaging

method, could be revealed, and the object image can be

achieved nonlocally

reference

Object beam

correlation：

Imaging using the 2nd order photon correlation:Fourier-transform Ghost Imaging with Hard X-rays@BL13W/SSRF

Experimental setup for X-ray FGI using

a pseudo-thermal X-ray sourcethe sample and an example of

intensity distribution pattern pairs

Diffraction patterns of the sample

obtained with 12.4keV X-raysThe sample’s amplitude distribution (a) and

phase distribution (b) in spatial domain

Hong Yu, et.al. Physical Review Letters, , 2016, 117(11)

Prof. HAN Shensheng’s group

Hong Yu, Ronghua Lu, Shensheng Han, Honglan Xie, Guohao Du, Tiqiao Xiao and Daming Zhu, Fourier-

transform ghost imaging with hard x-rays，Physical Review Letters 117, 113901 (2016).

TGISUM—real space ghost imaging

Reference arm

d

Detecting arm

d1 d2

Thermo source:

X-ray + sand paper

Pixel array

detector

Pixel array

detector

样品

Direct image Ghost image

Detector for the arm

with object taken as

bucket detector by

binning all the pixels

together

2nd order photon correlation X-ray imaging—leaf

Direct image

TGI

TGISUM

实验条件：P20000碳化硅砂纸,

同步辐射光源, 能量E=10keV

探测器分辨率: 0.65μm/pixel

曝光时间1s, 砂纸到探测器距离10cm, 样品贴在砂纸镜头盖上

Pixel array detector used for the object

arm. Spatial resolution info used

Can be used for low dose and quick imaging

Conclusion

• 2-D and 3-D X-ray imaging developed at SSRF with time resolution from ms-microsecond-nanosecond, and 2~25Hz for 3-D

• Movin contrast is useful for in operando imaging to complex system

• Real space ghost imaging may be employed for low dose and quick X-ray imaging

58

Thanks for your attention