BL01B1, BL14B2, BL32B2

A1

Production XAFS

Keywords: Versatile XAFS, Automated XAFS, Local
structure, Chemical state, Operando
X-ray absorption fine structure (XAFS) measures electronic states and the local atomic structure ofmatter. It is applicable to crystalline and amorphous materials, and has element selectivity that allows
analyses of materials with many different elements. In-situ measurements of reactions is also
possible. Automated systems for sequential measurements use robots for pellet fabrication. Our setup
is designed for safe and easy handling of reaction gases and heating cells for operando measurements
in catalytic chemistry.

• Features• Examples

Reaction gas feeder and in-situ
analysis of catalysts

Structural analysis of high-entropy alloy
nanoparticles using element selectivity

Pellet-fabrication robot for
XAFS measurement

5 mm
コンクリート100 um
アスファルト

20 mm

BL01B1

Y. Kuwahara et. al., J. Phys.
Chem. C 127, 4942 (2023).

N. Hashimoto et al.,JACS Au 3, 2131 (2023).

BL14B2• Towards SPring-8-II
The photon density at the sample position will be increased by a factor of 10 by improving
beamline optics. A high-count-rate fluorescence detector and a digital signal processor will
be installed to realize XAFS measurements of low-concentration samples in a much shortertime in collaboration with data science researches.

1

BL39XU, BL36XU, BL12XU
A2 X-ray emission spectroscopy/HERFD-XAFS/
X-ray Raman scattering Keywords: High-sensitivity chemical state analysis, Trace• Featureselement analysis, X-ray Raman scattering, RIXS

Our X-ray emission spectroscopy (XES) systems enables observation of fluorescent X-rays
allowing practical high-energy resolution fluorescence detected (HERFD) XAFS, which canobserve spectral fine structures and trace elements beyond the limits of conventional XAFS.
This captures tiny changes in chemical states (local structures, bonding states, valence,etc.) of specific elements, used in a variety of fields, condensed matter physics, catalytic
chemistry, and geo-environmental science.

• Examples High-sensitive X-ray
emission spectrometer

Spin transition under high pressure

Valence state analysis of dilute Eu by
HERFD-XAFS
Mn Kα1,2

Eu Lα1

Eu < 5 ppm

R. Konagaya, et al., Chem. Lett. 50, 1570 (2021).

Hard X-ray → Soft X-ray XAFS

✔ Up to 15 crystal can be mounted✔ Analyzer crystals are placed in a
vacuum chamberア• Towards SPring-8-II

Observation of Co 3d state under highpressure→ Verification of pressure-induced
spin crossover
Tsujimoto, et al., Sci. Rep. 6, 36253 (2016).

X-ray Raman scattering

Improvement of spectral acquisition technology with high energy resolution and sensitivity
will allow chemical state analysis of ultra-trace elements and observation of their electronic
states. Our method will contribute to discovery of rare metal resources and development of
next-generation functional materials using materials informatics through ultra-high2throughput measurements with ultra-high sensitivity.

A3

XAFS-CT

BL36XU, BL37XU, BL39XU, BL29XU

Keywords: Operando, Chemical state, Projection type,
Imaging type, High-speed scanning type
The Ccombination of X-ray imaging with XAFS or X-ray fluorescence visualizes 2D/3D distributions ofelements and their chemical states (local structures, bonding states), and is widely used in fuel cell
catalytic research and environmental science. Projection and imaging
measurements have been
extensively used to shorten the measurement time. Recently, development of on-the fly scanning has
enabled high-speed scanning commonly with fluorescence detectors with high-sensitivity and high countrate. Optical systems with variable magnification/reduction rates have been developed, leading to multiscale imaging and observations of trace elements.

• Features• Examples

Full-field microspectrometer

Visualization of electrode reactions inthin-film all solid state batteries

3D visualization of the degradation
progression of storage batteries

Full-field imaging
microspectrometer
Visualization of chemical
states in the cathode andanodelayersduringcharging and discharging
in the same field of view

✔ Projection CT with high speed and wide
field of view✔ High-resolution imaging CT→ High magnification with high efficiency

Full-field projection
microspectrometer
N. Ishiguro, et al.,ACS Appl. Energy Mater. 6, 8306 (2023).

When/where/how degradation
occurs in electrodes

Y. Kimura, et al., Small Methods, (2023).
DOI：10.1002/smtd.202300310• Towards SPring-8-II
Improvement of XAFS imaging for higher spatial resolution, higher throughput, and multiscale observation will realize highly efficient measurements of spatial distributions and time
variation of elements and chemical states. This will contribute to development of higher
functional materials by elucidation of mechanisms of chemical reactions. Collaboration with3
data-driven science will further develop 2D/3D spatial morphology and its kinetics.

A4

BL37XU、BL39XU、BL29XU

X-ray fluorescence, XMCD imaging

Keywords: Chemical state, Microstructure,
Element distribution• Features

X-ray fluorescence imaging, in which X-rays are focused to a small size are scanned on a sample andfluorescent X-rays are generated, can target a variety of elements and visualize element distributions
and chemical states with 100nm resolution. Imaging X-ray fluorescence microscopes using chromaticaberration-free mirror optics have been developed. X-ray magnetic circular dichroism (XMCD) imaging
measurement methods are available, enabling scanning microscopy and CT-based 2D/3D magnetic
domain structure observation.

• Examples X-ray fluorescenceimaging system

Visualization of quantification of anticancer
drug distribution in human tumor tissues

3D visualization of Skirmion
string by XMCD-CT

Scanning X-ray fluorescenceimaging system
Typicalhistopathology ofrectal cancer

5 mm

Imaging X-ray fluorescencemicroscope

S. Matsuyama et al., Opt. Express 27, 18318 (2019).

Scanning XRF
imagesLeft: Pt
Right: Fe
R. Koba et. al., Int. J. Cancer. 146, 2498 (2020).

S. Seki et al., Nat. Mater. 21, 181 (2022).

• Towards SPring-8-II
Innovations in focusing/imaging optics and detectors will realize high throughput imaging measurements,
leading to correlation analysis of microstructures of materials. Operando/in-situ measurements ofbatteries, catalysts, magnetic materials, and biological samples will be available. Combining this withmaterial informatics using databases and supercomputers will contribute to development of highly
functional materials and even environmental problems.

4

A5

Fast XAFS• Features

BL36XU

Keywords: QXAFS, Complex measurement,
Chemical state, Operando

X-ray absorption fine structure (XAFS) needs scanning X-ray energy and takes a long time
to complete element-selective measurements of chemical states and local structures. Our
system has a compact spectrometer that enables millisecond-order fast XAFS (QXASF)
used for tracking catalytic reactions of fuel cells. QXASF combined with X-ray diffraction(XRD) and projective imaging measures time dependence of 2D/3D distributions ofchemical states.

• Examples

QXAFS measurement
systemGalvano scan
Si 111/220 channel-cut
monochromator

Observation of oxygen
desorption reaction processes
Oxygen desorption reaction of
Sr3Fe2O7-δ
Simultaneous measurements
of XAFS/XRD→ Correlation between crystal
structures and chemical states✔ Fast XAFS(>20 ms)✔ Simultaneous
measurements of XRD,
projection imaging
Reference sample
for energy calibration

Spatial distribution of oxygen absorption
and release reaction of catalyst particles
Pt/Ce2Zr2Ox
QXAFS + Projection
imaging

酸素吸蔵
H. Matsui, et al.,Angew. Chem. Int. Ed., 55,
12022 (2016).
T. Yamamoto, et al.,Advanced Science 10, 2301876 (2023).

Oxygenrelease• Towards SPring-8-II
QXAFS measurements will be 100 times faster (order of microseconds) with higher
precision spectral measurements. This will realize tracking of high-speed evolution ofchemical reactions and local structures, acquiring multi-dimensional data, and establishingdatabase for reaction mechanisms through collaboration with data science technology sucn5
as Bayesian statistics and AI,

B1

BL09XU, BL46XU

Production HAXPES Keywords: Electronic state, Chemical state, Resonate HAXPES 3D• Features

space-resolved measurement, Automated HAXPES

Hard X-ray photoemission spectroscopy (HAXPES) non-destructively analyzes electronic states from thesample surface to the bulk (several tens of nm), and enables precise investigation of chemical bonding
and electronic states in the bulk and buried interfaces. Our system has elements/orbital-selective
methods called resonant HAXPES, which uses resonant excitation at the absorption edge, and 3D spaceresolved analysis using focused X-ray beams and angular-resolved measurements.

• Examples
Electrode surface-forming
species for storage batteries

Valence fluctuation phenomena inheavy electron systems

High throughput HAXPES system（sample chamber）

5 mm
コンクリート100 um
アスファルト20 mm

T. Hosaka et al., J. Mater. Chem. A, 8, 23766(2020).

E. Ikenaga et al., Synchrotron Radiat. News31, 10 (2018).

• Towards SPring-8-II

Upgrading the focusing optics will enable electronic-state mapping of practical materials
with high spatial resolution. Efficient analysis of multidimensional spectral data fromcontinuous measurements will become possible, including 3D space-resolved
measurements, energy scanning. Advanced analysis in a remote environment will be
performed in real time.

6BL09XU, BL46XU

B2• Features

Atmosphere control HAXPES Keywords: Electronic state, Operando,
Atmospheric pressure

Our hard X-ray photoemission spectroscopy (HAXPES) system has an atmospherecontrolled equipment for analyzing the electronic structures of samples under atmosphericpressure and specific atmospheres. This enables operando experiments under reactive
conditions and electronic structure analysis of absorbed species.

• Examples
Reaction mechanism of Pt catalysts
for fuel cells atmospheric pressure

Atmosphere controlled
HAXPES system

Evaluation of catalysts underreaction gas atmosphere

5 mm

Y. Takagi et al., Acc. Chem. Res., 51, 719 (2018).

T. Koitaya et al., J. Phys. Chem. C,
127, 13044 (2023).

• Towards SPring-8-II
High-precision HASPES in-situ and under operando conditions will enable measurements ofdevices and under gaseous atmosphere.
7

C1• Features

High resolution Compton scattering

BL08W

Keywords: Electron orbital states, Fermi surface

Electronic orbitals and Fermi surface are important for material properties. Lithium-ion
batteries, for example, have the redox properties determined by the electronic orbitals thattransfer electrons, while superconducting transitions, electric conduction and alloy
regularization are affected by the shape of Fermi surfaces. High-resolution Compton
scattering can visualize electron orbitals and Fermi surfaces, and extract related physicalobservables by measuring the electron density distribution in momentum space.

• Examples

Measurement of bulk states
without surface effects

Measurement under electromagnetic
fields and variable temperature

In situ measurement underambient conditions or in solution

Mechanism of anion charge
compensation（O2-/O-） of largecapacity cathode material
LixTi0.4Mn0.4O2

Visualization of hole states of highTc superconductor La2-xSrxCu4O4

Fermi surface and electronic
coherent length of random alloys
NiFeCoCrpy (a.u.)

Hole creatingsuperconductivity（underdoped）

p-type Mn t2g - O 2p orbitals
Nature 594, 213(2021)

Hole breaking
superconductivity（overdoped） 5 mm

1.5

1.5

1.0

1.0

0.5

0.5

0.0

0.0

-0.5

-0.5

-1.0

-1.0

-1.5
-1.5 -1.0 -0.5 0.0 0.5 1.0

px (a.u.)

1.5

コンクリートアスファルト20 mm-1.5-1.5 -1.0 -0.5 0.0 0.5 1.0 1.5

px (a.u.)

Science 332, 698 (2011)

Phys. Rev. Lett. 124, 046402 (2020)• Towards SPring-8-II
High-resolution Compton scattering can measure bulk electronic states without interrupted
by surface conditions. This method will promote fundamental understanding of themechanism of high-capacity Li ion batteries, and contribute to the development of carbonneutral materials.

8Magnetic Compton Scattering

C1

BL08

Keywords: Magnetic material, Magnetic property• Features

Magnetic materials are important components in industry including development of electricvehicles. The magnetism has its origin in quantum phenomena, but it is difficult toevaluate on a microscale because most experimental methods can only extract totalmagnetization. To measure physical observables directly related to the electronic
wavefunctions by spin states, magnetic Compton scattering is useful.

• Examples

Separated magnetization
measurement by magnetic quantum
number m

Magnetization measurement withseparated spin/orbital components

Electronic states by up/down spin

CoFeB(as prepared)

Magnetization (emu/cc)

500
0

|m|=0
|m|=1
|m|=2

(a)
-500
-2 -1 0

1

CoFeB(annealed)

500

Appl. Phys. Lett. 102, 082403 (2013)

2

Magnetization (emu/cc)

La1-xSrxMnO3
CoFeB/MgO
thin film
CoFeB/MgO(asprepared)

500

|m|=0
|m|=1,|m|=2

コンクリート0(c)-500-2 -1 0Light Sr-doping
・O p hole generated

1

2

H (T)
CoFeB/MgO(annealed)

500
J. Phys.: Condens. Matter 28, 436001 (2016)

20 mm

アスファルトHeavy Sr-doping
・O p hole broke down
・transition from up
spin Mn-3d to down
spin Mn-3d

Appl. Phys. Lett. 98, 052107 (2011)• Towards SPring-8-II00
Magnetic Compton scattering uses high-energy X-rays having excellent penetration that(b)(d)
enables evaluationof bulk properties-500-500 free from surface states. The new source will realize
high-speed mapping
materials/devices and at-2 -1of 0magnetic
1 2 properties-2 -1 inside
0 1 magnetic
2
interfaces.

9

C2

Nuclear Resonance Vibrational Spectroscopy- Active site of the enzyme -• Features

BL35XU, BL19LXU

Keyword: Element specific

Nuclear resonance vibrational spectroscopy is sensitive only to specific isotopes and provides information
about their vibrational states. It is particularly useful for enzymes, because it can extract the vibrationsof exactly the metals at the active center from a huge background. Combined with sophisticatedsimulations this provides valuable information about the structure of active centers of enzymes.

• Gallery
Average of 3 high impact (IF>12)
publications every year
List of recent publications[1] Nature Chem. Biol. (2023)
https://doi.org/10.1038/s41589-022-01226-w.
[2] Inorg. Chem. 62 (2023)[3] Faraday Discuss. 243 (2023).
[4] Biophys. J., 121 (2022) 346a.
[5] Proc. Natl. Acad. Sci. U.S.A., 118 (2021).
[6] J. Am. Chem. Soc., 143 (2021).
[7] Angew. Chemie Int. Ed., 60 (2021).
[8] J. Am. Chem. Soc., 143 (2021).
[9] Inorg. Chem., 60 (2021).
[10] Chem. Sci., 12 (2021).
[11] Biochemistry, 60 (2021).
[12] Angew. Chemie Int. Ed., 59 (2020).
[13] ACS Catal., 10 (2020).
[14] J. Am. Chem. Soc., 142 (2020).
[15] J. Am. Chem. Soc., 142 (2020).
[16] Chem. Sci., 11 (2020).

Active site in the enzymes

Enzyme for hydrogen: Hydrogenase

Elucidation of the Fe(IV)=O intermediatein the non-haem iron halogenase

Crucial insight into O2 stability
mechanisms in the active site of
the enzyme, hydrogenase

100 umコンクリート2H2 + O2 ↔ 2H2O

5 mm

アスファルトCatalytic cycle

20 mm

Energy states

Nature, 499 (2013) 320. doi:10.1038/nature12304

Angew. Chemie Int. Ed. 59, 16786 (2020).
https://doi.org/10.1002/anie.202005208• Toward SPring-8-II
Smaller samples will be possible with a small beam size at SP8-II. We also hope to
improve the resolution using the improved brilliance. Research of the artificial catalysts andmaterial science, especially earth science, will be accelerated by these features.

10

C2

Energy domain Mössbauer Spectroscopy- Complex materials -BL35XU, BL19LXU• Features

Keyword: Local electronic states
Energy domain Mössbauer spectroscopy at synchrotron radiation can investigate element-specific local
electronic states with small beam size and without radioisotopes. This technique is especially useful for
analyzing complex materials. Small beam size enable the study under the extreme conditions such as
high pressure and/or high temperature easily. Basically this is hyperfine spectroscopy but with a much
expanded range of resonances: e.g. Fe, Eu, Sm, Sn, Dy, K, Ge, Ni, Ir, Yb.

• Gallery
Charge fluctuations by 174Yb EDMS

Carbon Electrocatalysts by 61Ni EDMS

Synchrotron Mössbuer Source

Observation of the charge fluctuations
in a strange metal

Investigation of the Structure of
Atomically Dispersed NiNx Sites in Ni
and N-Doped Carbon Electrocatalysts

Synchrotron Mössbauer sourceof 57Fe is under developmentwith special device for public use

CO2 reduction on
Ni-N-C catalysts

5 mm
コンクリート100 um
アスファルト20 mm

Science 379, 908 (2023).
DOI: 10.1126/science.abc478

J. Am. Chem. Soc. 144, 21741 (2022).
https://doi.org/10.1021/jacs.2c09825

Work in prgress• Toward SPring-8-II
Better spatial resolution can be obtained due to the higher brilliance. A synchrotron
Mössbauer source of 57Fe is under development for the public use at SPring-8-II. We hopeto have a nm-scale beam size. Also, x-ray polarization analysis will become easier.

11

C2• Features

Time Domain Interferometry- Slow Dynamics -BL35XU, BL19LXU

Keyword: Slow dynamics
Time Domain Interferometry (TDI) gives us the information of nanoscale dynamics from nsec to µsec. It
can be applied to the soft materials such as ion liquid, ion conducting glass, rubber, liquid crystal andMembrane protein. This is basically the only alternative to Neutron Spin Echo (NSE) spectroscopy and isin fact better because it allows new access to materials with hydrogen and small samples.

• Gallery

Biomembranes

Energy and momentum region

Tire Rubber

Better understanding propertiesof biomembranes essential forlife activities
2H2 + O2 ↔ 2H2O

コンクリート100 um
アスファルトMicroscopic observation of the effects ofelongation on the polymer chain
dynamics of crosslinked polybutadiene

5 mm

20 mm

Phys. Rev. Lett. 127, 078102 (2021).
https://doi.org/10.1103/PhysRevLett.127.078102

J. Synchrotron Radiat. 29, 1180 (2022).
https://doi.org/10.1107/S1600577522007998• Toward SPring-8-II
Better spatial resolution can be obtained due to the higher brilliance. The gamma ray
quasi-elastic scattering in energy domain is also under development by SACLA/SPring-8
Basic Development Program.
12

C3

Thermal conduction and phonons BL35XU, BL43LXU• Features

Thermal conduction in solids is carried out by electrons and phonons. Thermoelectricmaterials are required to exhibit high electrical conductivity but low thermal conductivity.
Conversely, electrical insulators with high thermal conductivity are needed in, e.g.,
electronic circuits. In designing such materials, inelastic X-ray scattering is used toevaluate phonon properties. Such materials are sometimes synthesized in thin films,
where IXS is one of the few probes that may be utilized.

• Examples

Phonons in multilayers

Phonon Life time in ScN thin film

Kohn anomaly which is
not observed in balksamplesMultilayer thinfilm of
semiconductors
Phonon engineering
for thermo-electrics
Consistency
betweencalculations (red)and experiments(blue)
Appl. Phys. Lett. 110, 043102 (2017)

Kohn anomaly in supper lattice

Measuredphonon linewithsof ScN thin film
can be explained
3-phonon model.
Phys. Rev. Lett. 120, 235901 (2018)100 umAppl. Phys. Lett. 117, 111901 (2020)• Toward SPring-8-II
The high brilliance of SPring-8-II makes the measurements easier: the footprint the beamon the sample becomes smaller and the beam becomes more collimated. Consequently, it
more sophisticated experiments may be realized, and, in particular, the region of total
13
external reflection may be used to provide information with ~1nm sensitivity.

C3• Features

Dynamics of Complex Materials

BL35XU, BL43LXU

IXS serves a diverse community that investigates the interplay different degrees of
freedom in complex materials: the properties of many interesting and technologically.relevant materials arise from the interplay of lattice dynamics with electronic order,
magnetic order, structure and thermal condutivity. The small x-ray small beam size allows
investigations of phonons in samples that can not be measured by other methods.

• Examples

Common Softening in Cuprates

CDW instability, and related phonon
softening is present in multiple
families of cuprate superconductors

Phys. Rev. X 8, 011008 (2018)

Microscopic Mechanism of
Anti-Ferroelectricity

Electrons Stopping Phonons

Phonon softening and diffuse
scattering show antiferro-electricity
come from a missed phase transtion.

Combined structural/dynamics study
shows lone pair electrons cause
anharmonicity and reduced thermal
conductivity

Nature Comm. 4, 2229 (2013)

Angew. Chemie 62, e202218458 (2023)• Toward SPring-8-II
Smaller, faster, more extreme: The reduced beam size at SPring-8-II will make smaller
samples easier to measure and permit access to different and potentially more extreme(higher temperatures, high pressures) conditions.

14

C3

Dynamics of Disorder• Features

BL35XU, BL43LXU

Disorder remains one of the frontiers of science. Materials, such as liquids and glasses, that are notperiodic, are technologically important and poorly understood. At large length scales, they can betreated as continua, but as one approaches atomic length scales, the ”mesoscale”, such treatments
fail. Inelastic X-Ray scattering with extremely high resolution (𝚫E/E<10-7) provides a unique window
on this region, unmatched by any other technique. It promotes new understanding of the mesoscale,including both identification of commonalities in behavior and discovery of new scienfic concepts.

• Examples

Gas-like liquids and liquid-like gases

Space-Time View of Liquids

Liquid near thecritical point hasregions that are
dynamically
gas-like

A new approach show shows how
looking at dynamics directly inreal space allows on to gain inight– in this case the interaction ofneighboring water molecules
In water, thiscan be related
to the hydrogenbonds

Phys. Rev. Lett. 125, 256001 (2020)

Measuring where no one has measured befor
XIXS: Extreme Resolution IXS
0.38 meV FWHM
World leadingenergyresolution for
meso-scaleliquid dynamics
Flat Analyer @ 10m
Si(15 15 15) @ 29.66 keV<0.0002 K rms T control

Science Adv. 3 e1603079 (2017)100 umSamplePSD Area Detector
14x14 mm2, 55 um Pixel

Work in Progress• Toward SPring-8-II
Extreme resolution will bridge the gap: Despite great effort, there is now no technique that bridges
the gap between the length scale of ~60 nm (light scattering) and ~6 nm (IXS). The improved source
characteristics at SPring-8-II will allow IXS to approach the light-scattering limit and provide access todynamics that have been impossible to measure previously.
15

C3• Features

Deep Earth Investigations

BL35XU, BL43LXU

The detailed chemical composition and temperature conditions of the Earth’s interior are
constrained by comparing the density and elastic wave velocity of candidate materials
under high temperature and high pressure conditions in the laboratory with the observed
values of the Earth. In order to do so, the technique to measure precise velocities under
extreme conditions and pressure scales are required.

• Examples

Absolute pressure scale with single crystals

sound velocity at pressureof earth’s core

Elastic wave velocity of Fe-alloy liquid

Iron at 300 GPa, thepressure at the
inner core

J. Synchrotron Radiat. 15, 618 (2008)
Jpn. J. Appl. Phys. 56, 095801 (2017)
Comptes Rendus Geosci. 351, 236 (2019)
High Pressure Res. 40, 465 (2020)
J. Appl. Phys. 132, 055902 (2022)

Density andlongitudinalsound velocityof ironNature Comm. 13, 7211 (2022)

Silicon depleted outer core
deduced from the sound velocity
of Fe-Si alloy liquid
J. Geophys. Res. B 125, 019399 (2020)• Toward SPring-8-II
SPring-8-II will enable measurements of smaller samples and in more extreme conditions,allowing us to more close approach the conditions of Earth’s core16

C4

• Features

X-ray fluorescence holography

BL47XU

Keyword：3D atomic image

Holography has been widely used for 3D image reproduction in visible light, preventing
counterfeiting of banknotes etc. Our hard X-rays enables element-selective 3D atomic
images, which are used to analyze the local structure e.g. around specific additiveelements in crystals of semiconductors, or around metallic elements in proteins. Our
portable equipment having a large sample space is useful for detection and visualization oftiny deviations from the periodically ordered structures.

• Examples

Visualization of atomic displacement
around additive elements
Setup for X-ray fluorescence holography

Visualization of biosamples

Local structurenear dopantÅ
単位：Å

Hologram

Reconstructed
image

単位：Å

Tiny atomic displacement
by electric field

Determined the heme
slope with high accuracy

Heme structure of myoglobin• Towards SPring-8-II
Atomic scale visualization of intermediate phases between crystals and amorphous structures willcontribute to creation of new functional materials. Our nanobeam will visualize local structures andstructures within a single domain related to the functions of materials such as micron- and nano-sized
crystal grains, porous zeolites, as well as composite defects and in crystal-like glasses.

17

C5

• Features

Compton scattering imaging

BL08W, BL05XU

Keywords: Operando observation, Digital twin

Observation of a cross-section of the object without rotation is useful in analyzing the insideof a palm-sized object. A storage battery is built into a system and is difficult to rotate andobserve under operation. Compton scattering imaging enables non-destructive observation of
the inside of a sample without rotation.

• Examples
Observation of a crosssection of a battery without
rotating it
Li transfer

Sensitive to light elements
Internal structures of battery
products

Pt catalyst and water condensate
distribution inside fuel cells

CR123A

CR2032
ET=34ms

Simultaneous X-ray
fluorescence analysis ofheavy elements

ET=3s

コンクリートアスファルト20 mm
ET=34ms

ET=3s

J. Synchrotron Rad. 22, 161-164 (2015)

J. Synchrotron Rad. 28, 1174-1177 (2021).

Appl. Sci. 13(19), 10753 (2023)• Towards SPring-8-II
The new light source will enable high-speed observation that contributes to constructionsof digital twin products and validation of phenomenon simulators.
18

D1

BL13XU, BL19B2
Multi-purpose X-ray diffraction
Keywords: Multi-axis diffractometer, in-situ, operand• Features

measurement, mapping, customized

Our multi-purpose X-ray diffractometer has a large sample space, high load capacity, and a high degreeof freedom in angle and position control. Various X-ray scattering and diffraction measurements areavailable with selectable detectors. Setups include parallel optics, 0D + slit/spectroscopic crystal, 1D, and
2D at X-ray energies of 5-72 keV. Various sample environment control devices can be mounted on thesample stage such as in-situ observation (heating/cooling, tensile, light irradiation, etc.), operando
measurement (charging/discharging, voltage application, etc.), and mapping measurement of thin film,
bulk, and practical materials.

• Examples Multi-purpose 6-axis
X-ray diffractometer

Evaluation of crystallinity andorientation of organic thin films

Evaluation of microstructural changes inmetallic materials during deformation

Mechanism of
deformationin structural
materials

Determination ofdevicecharacteristics
I. Osaka, et al., J. Am. Chem. Soc. 2013, 135, 8834–8837• Towards SPring-8-II
High brilliance X-rays will accelerate the development of semiconductor devices, structural
materials, and various other practical materials through faster and more efficient operando
measurements as well as mapping measurements for analyzing mechanisms of
manufacturing processes.

19

X-ray Powder Diffraction

D2

BL13XU, BL02B2, BL19B2

Keyword: Automated measurement, Operando, Crystal structure analysis• Features

X-ray powder diffraction measures structures of crystals and their local properties. Our automatedsystem, sample preparation to measurements, provides high-quality data over a large area of reciprocal
space with high angular resolution. Short time measurements can be done even with small amounts,~mg, of sample. Operando measurements are available for fast phenomena, which are transient orrepetitive, with time resolution from seconds to milliseconds and in a variety of sample environments.

• Examples

Automated powder
diffraction system

Creation and utilization of large
volume and high quality data

Powder diffractometer

Gas storage materials
for hydrogen andexplosive gases

Next-generation magnets
using machine learning

Adv. Theory
Simul. 2023
Adv. Mater. 2021

Nat. Chem. 2022

Catalysts
automated sample
preparation

Zero-thermalexpansion materials

Adv. Mater. 2021

Observation of material
production processes
Ceramics production
processes

Adv. Mater. 2021
Nat. Rev. Mater. 2021

Batteries
Phase transition of
H-superionic conductors

JACS 2019
Nat. Commun. 2016

Operando observation of
decarbonization and newenergy materials
Operating behaviorof CO2 absorbent

Nat. Commun. 2020
Nat. Commun. 2023

Oxygen/hydrogen
reduction

Nature 2022

Water purification

Caffeine
purification

Nat. Mater. 2022

Bull. Chem.
Soc. Jpn. 2022

Novel materials
SPring-8
data center

Water-heavy water
separation

多元素ナノ合金
Science 2018

Adv. Sci. 2023

Langmuir 2021

• Towards SPring-8-II
The high-brilliance beam will increase the number samples to ~1000 samples/day. The high-quality
data automatically transferred to the data center, leading to next-generation DX with AI and materials
informatics (MI). Operando analysis will enable high-speed observation of micro regions with submillisecond time resolution. This will advance the understanding of various reaction processes.

20

D3

• Features

High-throughput PDF, in-situ PDF

BL04B2, BL08W, BL05XU

Keywords: Local structure, High-speed measurement

High-energy X-rays allow pair distribution function (PDF) analysis that gives quantitative data on local
distortion in materials. It has been applied to many research fields from earth science to industrial uses
such as rechargeable batteries and environmental catalysts. Our system offers high-throughput PDF
measurements that are 10-50 times faster than the conventional systems. High-precision in-situ PDF
measurements are also possible under extreme pressures such as those inside the earth.

• Examples

PDF measurement systems
7 sequential
detectors

Time-resolved
In situ測定デバイス

Next-generation
rechargeable batteries

Environment catalysts

Structure of V-based cathode materials
for rechargeable batteries without volume
changeVisualizing the mechanism of selective
catalysis induced by microwave

110 keV X線

High-throughput

High-energy X-ray
high-pressure

applicable to various
fields of research

Nature Mater.(2023)

Sci.
Adv.
(2023)

Structure of solid electrolyte incollaboration with Fugaku

Structure of materials forinexpensive photocatalysts

Energy Environ. Mater.(2023)

Nature Commun. (2022)

High-temperature fusion
In-situ measurement of molten
liquids forming to glass

Nature Commun. (2014)

Earth science
In-situ measurement of SiO2
under high pressure

Nature Commun. (2022)• Towards SPring-8-II
しInnovation of PDF analysis, including in-situ measurements, will be realized by a pinkbeam having 100 times higher flux, which accelerate materials development. Collaboration
with Fugaku supercomputer will establish ecosystems contributing to SDGs through further
development of material informatics (MI).

21

Fast/precise structure analysis• Features on micro single crystals
D4

BL05XU, BL02B1

Keywords: Precise structure analysis,High throughput
Single crystal structure analysis determines molecular and atomic structures, and is widely used inresearch on organic/inorganic materials, hybrid materials, and in drug discovery. Our technique using
micrometer size X-ray beams enables structure analysis of organic micro single crystals, precise
measurements of electronic density at high spatial resolution, and in-situ single crystal structure analysis
under external perturbations from light, heat, and pressure.

• Examples
Microcrystal
structure analyzer

Molecular structuresof functional materials

BL40XU

Precise structure
analysis system
BL02B1

Electron density distribution
at high-resolution
Precise analysis on density of Dirac
electrons in organic molecules

Microcrystal

100 umPhoto-induced molecular reactions

Valence electron density map of C60
Detector

X-ray energy is 50 keV（λ=0.248 Å)
Voids

Collimated X-ray beam of
micrometers

Heterogeneous radical pairstacking structures• Towards SPring-8-II
High-brilliance X-rays and a new 2D detector CITIUS will enable higher precision measurements ofsmaller, submicron, microcrystals. AI-equipped automatic micro single crystal sampling systems and sample
exchange robots will provide high throughput analysis of 150 micro single crystal per day, which is morethan 10 times what is possible now. This will allow more efficient searches for target materials and drug
discovery.

22

D5

• Features

keV)･BL13XU

Keywords：Lattice deformation, mapping

Zone plates and refractive lenses allow an x-ray beam to be focused down to sub-micron spot sizes,
enabling local analysis of crystal structures and lattice deformation. Our method has been used toanalyze lattice distortion caused by microstructure formation and strain distribution around latticedefects in semiconductors and related device materials. Recently the method has been extended tostructural materials and polymers.

• Examples
Experimental setup

Evaluation of local strain
inside semiconductor
microstructures
Evaluation of local strain
inside embedded
Ge1−xSnx/Ge microstructures（特注品）
150 μmン幅

Nanobeam X-ray diffraction/topography

FZP
CRLs
測長SEMによる計測値

81.7 nm1000 nm

98.83 mm

第一ゾーン直径
6978 nmIke et al.,Appl. Phys.
Lett. 106,
182104(2015).

Operando measurement by
time-resolved nano XRD
Analysis of lattice
deformation in AlGaN/GaN
by inverse piezo effect

H. Shiomi et al., Appl.
Phys. Express 14,095502 (2021).

Local crystal analysis
inside materials
Distribution of crystalline phases
inside concrete samples

A. Aili et al., J. Am.
Ceram. Soc. 105, 6924
(2022).

最外周ゾーン幅
80 nm• Towards SPring-8-II
The improved X-ray nanobeam intensity, 100 times higher than now, will enable mapping of a larger
number of samples including polycrystals and microcrystals in a short period of time. The nanobeam will
also be further miniaturized to achieve a resolution of several tens of nanometers. X-ray topography, as
a complimentary method, will also be further improved for digital topography with a large-angle camera
having a higher resolution.

D6• Features

XRD imaging/3DXRD

BL47XU, BL05XU

Key words: Grain, Orientation
mapping, Non-destructive, Operando

X-ray diffraction of microbeams may be used to identify the shape and orientation of individual grains of metallic materials
such as steel, aluminum alloys, and solder. Through statistical processing of intergranular orientation differences, grain shapes
etc., this method has revealed the nano-scale changes of matter disturbed mechanically by external forces, temperature
variations, and other factors. Utilizing high-energy X-rays with high transmission capability in the 100 keV range enables nondestructive analysis of the internal structure of practical material samples with ~ cm thicknesses.

• Features

Phase Transformation in Steel Materials

Non-destructive 3D nano-observation of Austenite
particle phase transformation in TRIP steel• Towards SPring-8-II

Toda et al., Acta
Mat. (2022).

Non-destructive Orientation Mapping Inside Iron Columns

Hayashi et al..
Non-destructive 3D mapping of grain orientations in a
Φ10 mm iron rod using 100 keV X-rays

The increased intensity of the focused beam of high-energy X-rays by a factor of 100 will reduce measurement from thepresent ~1/2 day to just a few minutes. This will enable routine measurements of many practical materials, contributing
significantly to the optimization of production processes.
24

D7• Features

Large-capacity high-pressure press

BL04B1, BL05XU

Keywords: Earth planet dynamics, Extreme condition

Measurements of crystal structures and physical properties under high pressure has become an
important method in industrial research, earth and planetary science, and for developing novel materials
such as high-Tc superconductors. Our large-capacity press system can perform precise X-ray diffraction
measurements of deformation and fracture dynamics under high hydrostatic pressure and uniform
heating environments. This method can reveal information such as micro-macro phenomena of samples
under highly controlled deviatoric stress.

• Examples

Earth and planetary
deep structures

Mechanism of earthquakes

Exploring new minerals
and metastable phases

High-pressure giantstrain processing

100 um• Towards SPring-8-II
The new source will enable measurements on millisecond timescales useful for understanding
phenomena such as astronomical collisions as well as more mundane but extremely important tasks likeobserving material processing and quality control. Application to investigating earthquakes andvolcanoes will give important social contributions. It will also enable 2D/3D mapping of chemicalcompositions and crystal structures of naturally heterogeneous samples.

25

E1

Production SAXS

• Features

BL19B2, BL40XU, BL40B2, BL05XU

Keywords：SAXS, USAXS, GI-SAXS, Automatedmeasurement, Operando measurement

Small angle X-ray scattering (SAXS) has been used for structural evaluation of mesoscopic objects (orderof 1nm to 100nm) such as microparticles, micelles and lamellae, inside materials. Our technique enables
operando measurements that track structural changes in situ during reaction processes. Ultra-small angle
X-ray scattering (USAXS) makes it possible to evaluate large and higher-order structures of 100nm suchas aggregates. Automated measurement systems used for a large of samples and GI-SAXS that measures
X-rays totally reflected near the sample surface are also available.

• Example

SAXS

Extract sample size, structure andsurface information

Automated SAXS
measurement system

USAXS
USAXS/SAXS
evaluation ofhierarchicalstructure
5 mm

Sample changer

コンクリート100 umAutomatic exchange
アスファルトof solution sample

20 mm

G.L. Hura et al., Nat. Meth. 6, 606 (2009)

Evaluation of long-period structure ofquasicrystals
M. Suzuki et al., ACS Nano 16, 6111 (2022)

Massive data analysis• Towards SPring-8-II
High-brilliance will reveal the formation mechanism of higher order structures that are essential in thefunctions of polymer materials through higher speed operando measurements of larger volume samples.
Promoting materials informatics using machine learning and compiling a database of a large numbers of
SAXS images will bring innovation to the utilization of X-ray scattering data.

26

BL40XU, BL40B2

E2

Imaging SAXS Keywords: Local structure analysis, Scattering CT,• Features

Simultaneous scattering imaging

Small angle X-ray scattering (SAXS) measures structural information of nano- and microscale structures inside samples. Combined with other techniques such as CT, SAXS can
extract local and/or 3D structural distribution by using microbeams.

• Example

Simultaneous scatteringand transmission imaging

microbeam SAXSSAXS-CT

Measurement of µm-sized carbon fibers

Combination of scattering measurementswith CT enables evaluation of distributionof parameters (size, period, shape) inside
samples.
oriented

WAXS

SAXS

boundary

5 mm

コンクリートnonoriented

107

100 um
アスファルト100

C. Zhu et.al. Carbon 235 (2012)
20 mm

Microbeam
analysis on toothremineralization

Schaff et al. Nature 527, 353 (2015)• Towards SPring-8-II
Improved brightness and high-speed detector CTIUS will reduce a measurement time of SAXS-CT from
10 hours to 10 minutes. A new system will reveal the distribution of nanoscale structures in real space
as well as averaged structural information. A large number of scattering and diffraction data of materials
with different manufacturing methods and compositions with matching analysis would be useful inmaterial development and forensic science.

27

Fast SAXS/XPCS

E3• Features

BL40XU, BL29XU

Keywords: Nonuniformity, Dynamics analysis, in-situ、in-vivo

Small angle X-ray scattering (SAXS) analyzes nano- and/or micron-scale structures inside samples. It
enables fast tracking of structural time evolution such as reaction processes during solution mixing,
sample deformation processes during tension and compression, and structural changes by temperature.
Hard X-rays with high transmission allow flexible environment around samples, as is relevant for in-vivo
and in-situ measurements. Coherent X-rays enable X-ray photon correlation spectroscopy (XPCS) thatmeasures sample hardening and softening processes due to changes in the internal structures.

• Example

Time-resolved SAXS

Rheology Scattering X-ray

XPCS

Orientation of liquid crystal
molecules by shear force
Phys. Chem. Chem.
Phys.,23:131 (2021)
100 um
アスファルトScience, 341, 1243
(2013)

Biochem. 55, 287(2015)

Tracking structural changes and synthesis
processes

5 mm

20 mm
Colloids & Surfaces A, 658, 130727 (2023)

Tracing structural changes of a sample
exhibiting viscoelasticity deformed byexternal forces.

Sci. Rep. 11, 9767 (2021).
Curing processes off epoxy resin.
The mesh structure changes withthe curing temperature.

• Towards SPring-8-II
Submillisecond resolution will be available for continuous measurements, and nanosecond
resolution for pup-probe methods, covering time scales from 10 -9 to 102 seconds. Highcoherent flux will enable speckle image analysis for local structures, and its temporalvariation will reveal the dynamics of density fluctuations and phase change processes.

28

F1

BL27SU, BL17SU

Soft X-ray XAFS

Keywords: Soft X-ray MCD,
Atmospheric pressure measurement
Soft X-ray XAFS enables observation of electronic states of light elements in organic materials andmetals in functional materials, and covers various research fields from condensed matter physics toenvironmental science. XAFS imaging is also available to investigate the disribution of elements and theirchemical states in high vacuum and in helium environments as well as ultra-high vacuum by using
differential pumping. A fast switching technology for circular polarizations and an electromagnet of up to
2T enable highly efficient measurements of SX-MCD, allowing investigation of magnetic properties ofsamples with elemental sensitivity.

• Features• Examples Soft X-ray XAFS
imaging system
Differential
pumping unit

Focusing optics(Zone plate)

Detector

Trace elements behavior
by XAFS imaging

Detection of magnetic octupoles
by SX-MCD

Scanning
microspectroscopy✔ Analysis ofcomposition ofminerals✔ Extraction of
trace elements→ 鉱物を構成する元素組成と硫黄との相関を可視化

Isaji et al., Prog Earth
Planet Sci. 6, 60 (2019).
Kimata et al., Nat. Commun. 12, 5582 (2021).

• Towards SPring-8-II
XAFS imaging with high spatial resolution and high throughput will realize highly efficientmeasurements of spatial and temporal variations of elements and chemical states, and also
contribute to revealing chemical reaction mechanisms. Collaboration with data-driven
science will give new insight to 2D/3D spatial morphology and its kinetics.
29

F2• Features

Soft X-ray photoemission
spectroscopy, ARPES

BL25SU
Keywords: Microbeam, Space resolved
measurements

Angle-resolved photoemission spectroscopy visualizes the motion of electrons as momentum-energy
distributions and the chemical/electronic states of functional materials. Our setup has micro-focused
intense soft X-rays that enable observation of electronic states in 3D momentum space with high energy
and angular resolution. A wide range of sample morphologies, including bulk crystals, thin films, andflakes, may be measured. Real-space-resolved measurements of electronic states using micro-focused
soft X-rays are also possible, as is useful for device performance analysis.

• Examples Micro-focused soft

X-ray ARPES system

Direct observation ofhalf-metallic band

Real-space resolved ARPES
measurement of silicon single crystals

Heusler alloys with difficult
cleavage

5 mm
コンクリートアスファルト20 mm

Spot size: 10x10 μm2
Energy resolution: E/ΔE < 20000
Temperature: 7 K ~ 300 K

Kono et al., Phys. Rev. Lett.,
125, 216403 (2020).

Muro, et al., J. Synchrotron Rad.
28, 1631 (2021).

• Towards SPring-8-II
Soft X-rays of > 100eV will be enhanced for establishment of a platform for 3D momentumresolved dynamics of electronic states. A denoising system using deep learning will be
installed for realizing ultra-high energy resolution with high throughput.
30

BL17SU、25SU
Soft X-ray imaging (Photoelectron
Keywords: Spectroscopic imaging, PEEM,• Features imaging type, scanning type)
SPELEEM, Nanobeam

F3Soft X-ray imaging visualizes light elements and their chemical state distributions, and is applicable tomagnets, semiconducting devices, dielectrics, strongly-correlated materials, biological samples, andorganic materials as is relevant for many research fields including material science, earth and planetaryscience, and forensic science. Scanning the focused beam and mapping the intensity of fluorescent Xrays and excitation current reveal rich information including elemental distribution, valence states, andmagnetic/charge orders at resolution of 10-10nm. Photoemission electro microscopy (PEEM) is alsoavailable that has high throughput data.

• Examples

Measurement system

PEEM

PEEM

Magnetic/charge domain
structure ofNiO(001)/Fe(1 nm)
heterojunction

Scanning soft X-ray microscope

Scanning soft X-ray
microscope
Chemical state analysis in
microscopic region using X-rays
focused several 100m
Thin, chip, and thick specimens
are available if their surface issmooth.
Possible analysis:
調整⽤ 試料・Low-vacuum
・He atmosphere
縦ナイフ・OperandoPD
横ナイフ
・Insulator

10 mm

試料ホルダー• Towards SPring-8-II
Possible detection of tiny elemental/magnetic signals and speeding up image acquisition
will improve effective spatial resolution. High flux beam with high throughput will elucidate
the mechanism of emergent functions and facilitate data mining by machine learning.

31

G1

BL20B2, BL28B2, BL05XU• Features

Prodution CT・Automated CT

Key words: mirco-CT

Non-destructive imaging by X-ray CT is widely used for medical, industrial, and security inspection.
SPring-8 enables high-spatial resolution CT images for thick samples by using intense, high-energy Xrays. Sophisticated X-ray cameras allow the FOV to several-cm with a pixel size below several microns.
Large and/or precious samples, even objects of cultural heritage, can be analyzed non-destructively, bysending them to SPring-8. Our automated CT instrument provides high-resolution 3D reconstruction
images. As it is non-destructive this can be useful as pre-analysis before conducting applying methods.

• Examples

Instrument

Fossil of a dinosaur(Fukuiraptor)

Cultural heritage

Soldering in power modules
Hayashi et al.

100 um5 mm

Dedicated capsule

Towards SPring-8-II

Lab X-raysourceSPring-8

Imai et al., JSR (2023).

Understanding the Rice Cultivation
Practices in the Yayoi Period from CT
Scans of Excavated Rice Blocks

Voids

Inamura et al., 作物研究 (2016).

The utilization of X-rays with high penetration capabilities will be enhanced. The captured data will be automaticallytransferred to the SPring-8 Data Center. This will facilitate advanced analyses such as 3D segmentation and functional analysis,
as well as Region of Interest (ROI) analysis for extracting specific areas of interest. Collaboration with th e 'Fugaku’supercomputer will contribute to various areas such as big data analysis of infrastructure materials, failure analysis ofcomponents and products, and the digitization and cataloging of fossils and cultural artifacts.

32

G2

BL20XU, BL47XU, BL29XU• Features

Nano CT/Ptychography Key words: Multiscale CT, Operando

X-ray CT enables the visualization of the 3D internal structure of objects. Our technique combines NanoCT and Micro-CT to visualize the interior of samples at a resolution of 100 nm for millimeter-sized
specimens. This technique, known as multi-scale CT, is particularly effective for high-energy X-rays
above 15 keV. Recent advancements in ptychography, utilizing coherence, have led to measurementswith high resolution below 10 nanometers. Applications are broad, including asteroid samples andneural cells through the depiction of intricate three-dimensional structures without disrupting the areasof interest.

• Examples

Particles from Asteroid Ryugu+50万サイクル

Nakamura et al., Science (2022).

Nanoscale Visualization of
Catalytic Functions
Hirose et al., Commun. Chem. (2019).

Direct Observation of Crack
Propagation in Titanium Alloy
Xue et al.,FFEMS (2022).

Various minerals and organic matter are present ina fine-grained matrix composed of layered
silicates. Voids within pyrrhotite and calcium
carbonate particles contain fluids such as H2O-CO2

Direct observation of ultra-high cycle
fatigue in Ti-6Al-4V. The initiation point of
fracture was identified, and theprogression of the fracture was captured.

5 mm

Ptychography XAFS-CT enabled to visualize
the 3D distribution of oxidation states incatalytic particles at the nanoscale• Towards SPring-8-II
Higher brightness resulting in higher spatial resolution and phase sensitivity in nano-CT fills the resolution gap withtransmission electron microscope CT (TEM-CT), and enables 3D observations at various scales. The research areas would
expand into biomimetics, unraveling and utilizing the 3D microstructures and functions in living organisms. Fully coherent
X-rays and the CITIUS detector will realize ptychography measurements with sub-nanometer resolution on a routine
basis, enabling nano-level measurements of crucial materials such as semiconductors.

33

G3

• Features

BL20B2, BL47XU, BL05XU
High-speed imaging & CTKey words: Operando
CT、High-speed movie

High-speed cameras for the visible light cannot access the interior of objects. At SPring-8, intense Xrays and high-speed X-ray cameras enable high-speed video recording and operando CT measurementsof transient or repetitive fast phenomena with a time resolution ranging from milliseconds tomicroseconds. This capability enables the detailed capture of rapid deformations inside objects, themechanisms of processing, and the movement of biological entities. Our technique is applicable to awide range of fields such as material development, engineering and medicine.

• Examples

Deterioration due to High-Speed
Deformation in Rubber

Observation of the Metal Melting
and Solidification Process

Understanding the Principles ofPrecision Machining Processes

Mimura et al.

Mashita et al., JSR (2021).

Observation of metal melting andsolidification phenomena induced by laser
heating at speeds exceeding 10 kHz.

Elucidating the principles of various precision
machining processes through ultra-high-speed,
non-destructive measurements at the order of
10,000 fps• Towards SPring-8-II
Improved brightness, temporal and spatial resolution will enable microsecond timescale analysis for submicron regions. This will contribute to ultra-precise and high-speed advancement of manufacturing by
revealing the true principles behind conventional phenomena such as material processing, fracture, anddielectric breakdown.

34

H1

• FeaturesProtein Crystallography(Single Crystal Diffractometer)

BL26B1, BL32XU, BL41XU, BL45XU

Keyword: Automated measurement

X-ray protein crystallography is a fundamental technique in structural biology and drug discovery.
High-brilliance X-rays, sample exchange robots, and high-speed detectors with high sensitivity make itpossible to obtain high-resolution data in a short period. Frozen crystal samples housed in worldstandard sample pins and cassettes can be sent to us for automated or remote measurement. Ultrahigh resolution measurements using short X-rays (~30 keV) are also available.

• Examples

Automated diffractometer

ZOO system for automatedmeasurement

High resolution measurement by
short wavelength diffraction

100 um

5 mm

Sampleloading

Takaba et al., Sci Rep 7,43162 (2017)

Takaba et al., IUCrJ 6,
386-400 (2019)• Towards SPring-8-II
Serial measurements with high-brilliance microbeam will expand the number of samples andpromote higher precision in automated appraoches, including faster screening required for drug
discovery and synthetic biology. Improvement of our techniques will contribute to high-precision
analysis using a diffractometer for biopolymers in combination with other quantum beam probes.

35

H2

Correlative structural analysis• Features

OthersKeywords: Single particle analysis, character evaluation,
Cryo-TEM

Structural analysis of biopolymers has become increasingly diversified. Correlative structural analysis
combined with multiple measurement methods can reveal more detailed molecular behaviors.
CryoTEM and BioSAXS techniques enable character evaluation of samples that are difficult tocrystallize. Our experimental environment includes everything from sample production to data
analysis, and will support efficient sample preparation and diffraction measurement with crystallization
plates.

• Examples

Structural Analysis Pipeline

Crystal preparation environment
and evaluation measurements

CryoTEM

Membrane protein complex
analyzed by CryoTEM

Crystal sample preparation facility
EM01CTJEOL
CRYO ARM 300

Plate diffractometer

Structure of gastric proton channel andinhibitor complex analyzed by CryoTEM• Towards SPring-8-II
To promote multifaceted structural studies of biopolymers, user support will be provided by using
CryoTEM and bioSAXS in combination with dynamical crystal structure analysis. Development of an
integrated environment from the preparation of target samples optimized for each method willaccommodate the various measurement methods that become available via the increased beamline
performance.

36

H3

BioSAXS• Features

BL40B2, BL38B1

Keywords: SEC-SAXS, Dynamical analysis

BioSAXS is a method to analyze the solution structure of biopolymers such as proteins. High intensity
X-rays enable short-time measurements of structures under dilute conditions. Our high-precision
detectors for narrow X-ray beams have achieved high resolution in small angles scattering and areused in many research fields from academia to industry. The SEC-SAXS method is also available, inwhich measurement cells are connected to gel filtration chromatography for protein separation. This
technique gives monodisperse solutions and their components may be analyzed even fromsolutions mixtures of various molecular sizes.

• Examples Size-exclusion chromatography
coupled SAXS system

SEC-Column

Dynamical
structure analysis

Automated measurement
and analysis

Pump-probe method (ns - μs)

100 umStopped-flow method (ms)Automatic measurements bysolution exchange robot• Towards SPring-8-II

Higher-quality, higher-brilliance X-ray beams will enable comprehensive measurements under various
conditions (concentration, temperature, pH, ligand concentration). They will also realize titration-type
SAXS, high time-resolution, and scattering measurements over a wide angular range. Combinationsof these methods with other experimental methods will further improve functional analysis such as
dynamical properties of samples.

37

H4

• Features

BL41XU, BL26B1
Dynamical Crystal Structure Analysis
Keywords: Time-resolved measurement,
at Room Temperature
Structural polymorphism Serial crystal

structure analysis
Protein crystallography has revealed an importance of dynamical properties at room temperature,especially by using XFEL. Our experimental systems offer serial measurements for dynamical crystal
structure analysis that enables detection of diffraction data in various delay time from possible statesof reacting processes induced by light irradiation or substrate addition. Diffraction measurements withcrystallization plates are also available.

• Examples

Dynamical structure analysis using
serial crystallography

Measurement at room temperature – HAG method

Structural analysis targeting time resolution of msec-sec• Time-resolved measurement system using laser excitation
incorporating the injector system developed at SACLA• Development of serial synchrotron crystallography (SSX) techniques

Water-soluble polymer coating andtemperature/humidity control• temperature(4-70℃), humidity(50-100%RH),
pH change available• Application to microspectroscopy and photoexcitation
Crystal mounting method

5 mm
Dynamical structure analyzing system
Fixed serial target method
sample holder

X-rayinkjetStructural changes due totemperature changes

matrixprotein crystal

Structural changes
due to humidity
changesmatrix added crystal• Towards SPring-8-II
Our pink beam technology provides more than two orders of magnitude increase in intensity. A
microbeam will enable even smaller crystals and time-resolved measurements on the order ofmicroseconds. It will also enable dynamic structural genomics and lead to applications such as
structure-based drug discovery, including transition structure information.

38