BL03HB: a Laue microdiffraction beamline for both protein crystallography and materials science at SSRF

A Laue microdiffraction beamline (BL03HB) was constructed at the Shanghai SynchrotronRadiation Facility (SSRF). This beamline featu res two consecutive focusing points in twodifferent sectors within its end station, the first dedicated to protein crystallography and theother tailored to materials science applications. Based on a superbend dipole magnet with amagnetic field of 2.29 T, a two-stage focusing design was implemented with two sets of Kirkpatrick- Baez mirrors to achieve a micro white beam as small as 4.2 um X4.3 pμm at the firstsector and 09 pum X 1.3 pum at the second sector in the standard beamline operation mode at SSRF.The X-ray microbeam in the two sectors can be easily switched between monochromatic andwhite beams by moving a four-bounce monochromator in or out of the light path, respectively. Inthe protein crystallography sector, white-beam Laue microdifraction was dermonstrated tosuccessully determine the structure of protein crystals from only a few images of diffraction data .collected by a Pilatus 2 M area detector. In the materials science sector, the white -beam Lauediffraction was collected in a reflection geometry using another Pilatus 2 M area detector, whichcould map the microstructural distribution on the sample surface by scanning the samples. Ingeneral, the BL03HB beamline promotes the application of Laue microdiffraction in both proteincrystallgraphy and materials science. This paper presents a comprehensive overview of theBL03HB beamline, end station, and the first commission results.

Identification of optimal composition with superior electrochemical properties along the zero Mn^(3+)line in Na_(0.75)(Mn-Al-Ni)O_(2)pseudo ternary system

Biphasic layered oxide cathodes,known for their superior electrochemical performance,are prime candidates for commercializing in Na-ion batteries.Herein,we unveil a series of P3/P2 monophasic and biphasic Al-substituted Na_(3/4)Mn_(5-x/8)Al_(2x/8)Ni_(3-x/8)O_(2)layered oxide cathodes that lie along the‘zero Mn^(3+)line’in the Na_(3/4)(Mn-Al-Ni)O_(2)pseudo-ternary system.The structural analysis showed a larger Na^(+)conduction bottleneck area in both P3 and P2 structures with a higher Al3+content,which enhanced their rate performance.In each composition,the P3/P2 biphasic compound with nearly equal fractions of P3 and P2 phases outperformed their monophasic counterparts in almost all electrochemical performance parameters.Operando synchrotron XRD measurements obtained for the monophasic P3 and biphasic P2/P3 samples revealed the absence of the O3 phase during cycling.The high structure stability and faster Na^(+)transport kinetics in the biphasic samples underpins the enhancement of electrochemical properties in the Al-substituted P3/P2 cathodes.These results highlight fixed oxidation state lines as a novel tool to identify and design layered oxide cathodes for Na-ion batteries in pseudo-ternary diagrams involving Jahn-Teller active cations.

High-precision X-ray polarimeter based on channel-cut crystals

We report on using synthetic silicon for a high-precision X-ray polarimeter comprising a polarizer and an analyzer,each based on a monolithic channel-cut crystal used at multiple Brewster reflections with a Bragg angle very close to 45°.Experiments were performed at the BL09B bending magnet beamline of the Shanghai Synchrotron Radiation Facility using a Si(800)crystal at an X-ray energy of 12.914 keV.A polarization purity of 8.4×10^(-9)was measured.This result is encouraging,as the measured polarization purity is the best-reported value for the bending magnet source.Notably,this is the firstly systematic study on the hard X-ray polarimeter in China,which is crucial for exploring new physics,such as verifying vacuum birefringence.

Time-resolved ultra-small-angle X-ray scattering beamline(BL10U1)at SSRF

The construction of a new beamline,BL10U1,was completed at the Shanghai synchrotron radiation facility in 2020.This multipurpose beamline was designed to provide X-ray scattering techniques such as ultra-small-angle X-ray scattering(USAXS),small-angle X-ray scattering(SAXS),wide-angle X-ray scattering,and microfocus SAXS(μSAXS)for a broad user community.To realize fast time-resolved USAXS experiments,the beamline adopted an in-vacuum undulator with a total length of 1.6 m as the photon source.An in-house cryogenic-cooled double multilayer monochromator was installed to deliver a photon flux of approximately 10^(13) photons/s at a photon energy of 10 keV.The three-year successful operation of this beamline demonstrated that the monochromator operated smoothly,as expected.BL10U1 has three end stations in succession:USAXS end station,μSAXS end station,and end station for industrial applications.The minimum scattering vector q~0.0042 nm^(-1) at 10 keV can be achieved at the USAXS end station equipped with a 28 m-long and 1.8 m-diameter vacuum flight tube.At theμSAXS end station,a beam spot of less than 10×8μm was achieved for micro-SAXS experiments.In contrast,in situ experimental instruments up to 5 m high and 8 m wide can be mounted at the industrial application end station,which offers industrial scientists the opportunity to use their large industrial equipment.BL10U1 opens up a new capability to investigate phenomena such as non-equilibrium and dynamic processes of materials with a wide length scale from angstroms to micrometers with millisecond time resolution.In this paper,we also report beamline design considerations and commissioning results.

Microstructures and micromechanical behaviors of high -entropy alloys investigated by synchrotron X-ray and neutron diffraction techniques: A review

High-entropy alloys(HEAs)possess outstanding features such as corrosion resistance,irradiation resistance,and good mechan-ical properties.A few HEAs have found applications in the fields of aerospace and defense.Extensive studies on the deformation mech-anisms of HEAs can guide microstructure control and toughness design,which is vital for understanding and studying state-of-the-art structural materials.Synchrotron X-ray and neutron diffraction are necessary techniques for materials science research,especially for in situ coupling of physical/chemical fields and for resolving macro/microcrystallographic information on materials.Recently,several re-searchers have applied synchrotron X-ray and neutron diffraction methods to study the deformation mechanisms,phase transformations,stress behaviors,and in situ processes of HEAs,such as variable-temperature,high-pressure,and hydrogenation processes.In this review,the principles and development of synchrotron X-ray and neutron diffraction are presented,and their applications in the deformation mechanisms of HEAs are discussed.The factors that influence the deformation mechanisms of HEAs are also outlined.This review fo-cuses on the microstructures and micromechanical behaviors during tension/compression or creep/fatigue deformation and the application of synchrotron X-ray and neutron diffraction methods to the characterization of dislocations,stacking faults,twins,phases,and intergrain/interphase stress changes.Perspectives on future developments of synchrotron X-ray and neutron diffraction and on research directions on the deformation mechanisms of novel metals are discussed.

High-precision X-ray characterization for basic materials in modern high-end integrated circuit

Semiconductor materials exemplify humanity's unwavering pursuit of enhanced performance,efficiency,and functionality in electronic devices.From its early iterations to the advanced variants of today,this field has undergone an extraordinary evolution.As the reliability requirements of integrated circuits continue to increase,the industry is placing greater emphasis on the crystal qualities.Consequently,conducting a range of characterization tests on the crystals has become necessary.This paper will examine the correlation between crystal quality,device performance,and production yield,emphasizing the significance of crystal characterization tests and the important role of high-precision synchrotron radiation X-ray topography characterization in semiconductor analysis.Finally,we will cover the specific applications of synchrotron radiation characterization in the development of semiconductor materials.

Quick-scanning X-ray absorption fine structure beamline at SSRF

The layout and characteristics of the hard X-ray spectroscopy beamline(BL11B)at the Shanghai synchrotron radiation facility are described herein.BL11B is a bending-magnet beamline dedicated to conventional and millisecond-scale quick-scanning X-ray absorption fine structures.It is equipped with a cylindrical collimating mirror,a double-crystal monochromator comprising Si(111)and Si(311),a channel-cut quick-scanning Si(111)monochromator,a toroidal focusing mirror,and a high harmonics rejection mirror.It can provide 5-30 keV of X-rays with a photon flux of~5×10^(11)photons/s and an energy resolution of~1.31×10^(-4)at 10 keV.The performance of the beamline can satisfy the demands of users in the fields of catalysis,materials,and environmental science.This paper presents an overview of the beamline design and a detailed description of its performance and capabilities.

Novel high-voltage cathode for aqueous zinc ion batteries:Porous K_(0.5)VOPO_(4)·1.5H_(2)O with reversible solid-solution intercalation and conversion storage mechanism

Cathode materials that possess high output voltage,as well as those that can be mass-produced using facile techniques,are crucial for the advancement of aqueous zinc-ion battery(ZIBs)applications,Herein,we present for the first time a new porous K_(0.5)VOPO_(4)·1.5H_(2)O polyanionic cathode(P-KIVP)with high output voltage(above 1.2 V)that can be manufactured at room temperature using straightforward coprecipitation and etching techniques.The P-KVP cathode experiences anisotropic crystal plane expansion via a sequential solid-solution intercalation and phase co nversion pathway throughout the Zn^(2+)storage process,as confirmed by in-situ synchrotron X-ray diffraction and ex-situ X-ray photoelectron spectroscopy.Similar to other layered vanadium-based polyanionic materials,the P-KVP cathode experiences a progressive decline in voltage during the cycle,which is demonstrated to be caused by the irreversible conversion into amorphous VO_(x).By introducing a new electrolyte containing Zn(OTF)_(2) to a mixed triethyl phosphate and water solution,it is possible to impede this irreversible conversion and obtain a high output voltage and longer cycle life by forming a P-rich cathode electrolyte interface layer.As a proof-of-concept,the flexible fiber-shaped ZIBs based on modified electrolyte woven into a fabric watch band can power an electronic watch,highlighting the application potential of P-KVP cathode.

Infrared microspectroscopy beamline BL06B at SSRF

The infrared microspectroscopy beamline(BL06B) is a phase Ⅱ beamline project at the Shanghai Synchrotron Radiation Facility(SSRF). The construction and optical alignment of BL06B were completed by the end of 2020. By 2021, it became accessible to users. The synchrotron radiation infrared(SRIR) source included edge radiation(ER) and bending magnet radiation(BMR). The extracted angles in the horizontal and vertical directions were 40 and 20 mrad, respectively. The photon flux, spectral resolution, and focused spot size were measured at the BL06B endstation, and the experimental results were consistent with theoretical calculations. SRIR light has a small divergence angle, high brightness, and a wide wavelength range. As a source of IR microscopy, it can easily focus on a diffraction-limited spatial resolution with a high signal-to-noise ratio(SNR). The BL06B endstation can be applied in a wide range of research fields, including materials, chemistry, biology, geophysics, and pharmacology.

Ultrahard X-ray multifunctional application beamline at the SSRF

The ultrahard X-ray multifunctional application beamline(BL12SW)is a phase-II beamline project at the Shanghai Syn-chrotron Radiation Facility.The primary X-ray techniques used at the beamline are high-energy X-ray diffraction and imaging using white and monochromatic light.The main scientific objectives of ultrahard X-ray beamlines are focused on two research areas.One is the study of the structural properties of Earth’s interior and new materials under extreme high-temperature and high-pressure conditions,and the other is the characterization of materials and processes in near-real service environments.The beamline utilizes a superconducting wiggler as the light source,with two diamond windows and SiC discs to filter out low-energy light(primarily below 30 keV)and a Cu filter assembly to control the thermal load entering the subsequent optical components.The beamline is equipped with dual monochromators.The first was a meridional bending Laue monochromator cooled by liquid nitrogen,achieving a full-energy coverage of 30-162 keV.The second was a sagittal bending Laue monochromator installed in an external building,providing a focused beam in the horizontal direction with an energy range of 60-120 keV.There were four experimental hutches:two large-volume press experimental hutches(LVP1 and LVP2)and two engineering material experimental hutches(ENG1 and ENG2).Each hutch was equipped with various near-real service conditions to satisfy different requirements.For example,LVP1 and LVP2 were equipped with a 200-ton DDIA press and a 2000-ton dual-mode(DDIA and Kawai)press,respectively.ENG1 and ENG2 provide in situ tensile,creep,and fatigue tests as well as high-temperature conditions.Since June 2023,the BL12SW has been in trial operation.It is expected to officially open to users by early 2024.

Insights into the hydrogen evolution reaction in vanadium redox flow batteries:A synchrotron radiation based X-ray imaging study

The parasitic hydrogen evolution reaction(HER)in the negative half-cell of vanadium redox flow batteries(VRFBs)causes severe efficiency losses.Thus,a deeper understanding of this process and the accompanying bubble formation is crucial.This benchmarking study locally analyzes the bubble distribution in thick,porous electrodes for the first time using deep learning-based image segmentation of synchrotron X-ray micro-tomograms.Each large three-dimensional data set was processed precisely in less than one minute while minimizing human errors and pointing out areas of increased HER activity in VRFBs.The study systematically varies the electrode potential and material,concluding that more negative electrode potentials of-200 m V vs.reversible hydrogen electrode(RHE)and lower cause more substantial bubble formation,resulting in bubble fractions of around 15%–20%in carbon felt electrodes.Contrarily,the bubble fractions stay only around 2%in an electrode combining carbon felt and carbon paper.The detected areas with high HER activity,such as the border subregion with more than 30%bubble fraction in carbon felt electrodes,the cutting edges,and preferential spots in the electrode bulk,are potential-independent and suggest that larger electrodes with a higher bulk-to-border ratio might reduce HER-related performance losses.The described combination of electrochemical measurements,local X-ray microtomography,AI-based segmentation,and 3D morphometric analysis is a powerful and novel approach for local bubble analysis in three-dimensional porous electrodes,providing an essential toolkit for a broad community working on bubble-generating electrochemical systems.

NEUTRINO BEAM LINES AT HIGH-ENERGY PROTON SYNCHROTRONS

Revised September 2013 with numbers verified by representatives of the synchrotrons （contact C.-J. Lin, LBNL）. For existing （future） neutrino beam lines the latest achieved （design） values are given.

ARCADE 2 Spatial Roar, What Theory of Relation Reveals

The theory of Relation provides an explanation for the Arcade 2 excess. It assumes that the isotropic radio emission measured by the Arcade 2 Collaboration, which is 5 - 6 times brighter than the expected contributions from known extra-galactic sources, is the residue of an immense primitive energy of ordinary matter released by a relativistic bang almost 100 million years after the big bang, which gave the mass-energy the missing gravity to activate contraction. This relativistic bang, via a Lorentz energy transformation, would have released enormous energy held to be the source of the powerful radio noise detected by the NASA researchers. This transformation would have simultaneously triggered the formation of the first stars from dense gas and the reionization of less dense neutral gas. This departs from the idea that continuous reionization began after the formation of the first stars. We emphasize the importance of primordial magnetic fields, which would have generated significant density fluctuations during recombination and acted as a direct seed for cosmic structures. The first stars and galaxies were bathed in strong magnetic fields that gave rise to the radio microwave din (boom) discovered by Arcade 2. These intense magnetic fields alter the trajectory of charged particles zooming near the speed of light, triggering the space roar and emitting radiation that forms a synchrotron radio background. The theory of Relation offers an alternative to the Lambda-CDM cosmological model, which has become the standard model of the big bang, which leads straight to the vacuum catastrophe.

Study of a magnetic alloy-loaded cavity for compact synchrotrons

Magnetic alloy（MA）-loaded cavities have been widely used in compact proton and heavy-ion synchrotrons,and the MA core is the key issue in their development.Chinese-produced MA has never yet been adopted as core material for an MA-loaded cavity.To use Chinese-produced MA as the core material,it is necessary to study its properties,and compare with MA material produced elsewhere.In this paper,the properties of several MA cores made of Chinese-produced material are measured.Based on the measured results,a schematic design is produced for a cavity which could obtain 1 kV gap voltage with less than 1.5 kW power dissipation in the frequency range of0.5-7 MHz.The difference between resonant frequencies obtained from simulation and analytical results is less than10%.

SAPT:a synchrotron-based proton therapy facility in Shanghai

Because of its excellent dose distribution,proton therapy is becoming increasingly popular in the medical application of cancer treatment.A synchrotron-based proton therapy facility was designed and constructed in Shanghai.The synchrotron,beam delivery system,and other technical systems were commissioned and reached their expected performances.After a clinical trial of 47 patients was finished,the proton therapy facility obtained a registration certificate from the National Medical Products Administration.The characteristics of the accelerator and treatment systems are described in this article.

Dynamically-evolved surface heterojunction in iridium nanocrystals boosting acidic oxygen evolution and overall water splitting

Simultaneously realizing improved activity and stability of acidic oxygen evolution reaction(OER) electrocatalysts is highly promising for developing cost-effective sustainable energy in the splitting of water technique.Herein,we report iridium nanocrystals embedded into 3D conductive clothes(Ir-NCT/CC) as a low iridium electrocatalyst realizing ultrahigh acidic OER activity and robust stability.The well-designed Ir-NCT/CC requires a low overpotential of 202 mV to reach the current density of 10 mA cm^(-2)with a high mass activity of 1754 A g^(-1).Importantly,in acidic overall water splitting,Ir-NCT/CC merely delivers a cell voltage of 1.469 V at a typical current density of 10 mA cm^(-2)and also maintains robust durability under continuous operation.We identify that a low working voltage drives the formation of a highly stable amorphous IrOxactive phase over the surface of Ir nanocrystals(surface heterojunction IrOx/Ir-NCT) during operating conditions,which contributes to an effective and durable OER process.

The 3D nanoimaging beamline at SSRF

Full-field transmission X-ray microscopy(TXM)is a powerful non-destructive three-dimensional(3D)imaging method with a nanoscale spatial resolution that has been used in most synchrotron facilities worldwide.An in-house-designed TXM system was constructed at the BL18B 3D nanoimaging beamline at the Shanghai Synchrotron Radiation Facility.The beamline operates from 5 to 14 keV and enables 20 nm spatial resolution imaging.The characterization details of the beamline are described in this paper.The performances in terms of spatial resolution,nano-CT,and nano-spectral imaging of the TXM beamline are also presented in this article.

Understanding Pseudocapacitance Mechanisms by Synchrotron X-ray Analytical Techniques

Pseudocapacitive materials that store charges via reversible surface or near-surface faradaic reactions are capable of overcoming the capacity limitations of electrical double-layer capacitors.Revealing the structure–activity relationship between the microstructural features of pseudocapacitive materials and their electrochemical performance on the atomic scale is the key to build high-performance capacitor-type devices containing ideal pseudocapacitance effect.Currently,the high brightness(flux),and spectral and coherent nature of synchrotron X-ray analytical techniques make it a powerful tool for probing the structure–property relationship of pseudocapacitive materials.Herein,we report a comprehensive and systematic review of four typical characterization techniques(synchrotron X-ray diffraction,pair distribution function[PDF]analysis,soft X-ray absorption spectroscopy,and hard X-ray absorption spectroscopy)for the study of pseudocapacitance mechanisms.In addition,we offered significant insights for understanding and identifying pseudocapacitance mechanisms(surface redox pseudocapacitance,intercalation pseudocapacitance,and the extrinsic pseudocapacitance phenomenon in battery materials)by combining in situ hard XAS and electrochemical analyses.Finally,a perspective for further depth of understanding into the pseudocapacitance mechanism using synchrotron X-ray analytical techniques is proposed.

Commissioning and operation of the cryostat for 3W1 SC wiggler

A 3W1 superconducting wiggler(SCW)with the pole gap of 68 mm was successfully tested and installed in a BEPC II storage ring in November,2019.The goal of zero liquid helium consumption was achieved,and the cryogenic system exhibited a 12%residual cooling capacity(approximately 0.69 W@4.2 K).The 3W1-SCW was set to operate at 2.49 T and has been operating for more than seven months.Three instances of magnet quenching occurred during the normal operation.The evaporated helium gas can be recycled to the helium gas recycling system when the pressure in the helium tank is higher than the parameter value(the setpoint of the pressure value is 1.2 bara).The cryogenic system can be recovered within 4 h if sufficient liquid helium is available to inject into the cryostat.

The effect of temperature on load partitioning evolution in magnesium metal matrix composite reinforced with Ti particles using in-situ synchrotron radiation diffraction experiments

The load partitioning between the magnesium and titanium phases in an extruded Mg-15%Ti(vol.%) composite from room temperature up to 300 ℃ using synchrotron radiation diffraction during in-situ compression tests. During compression, the magnesium matrix composite deforms mainly by the activation of the extension twinning system up to 200 ℃. The volume fraction of twins increases with the plastic strain but decrease with the compression temperature. Hard titanium particles bear an additional load transferred by the soft magnesium matrix from room temperature up to 300 ℃. This effect is amplified after yield stress during plastic deformation. Additionally, twins within magnesium grains behaves as an additional reinforcement at low temperature(below 200 ℃) inducing an increase in the work hardening of the composite.