Exploring battery material failure mechanisms through synchrotron X-ray characterization techniques

Rechargeable battery cycling performance and related safety have been persistent concerns.It is crucial to decipher the capacity fading induced by electrode material failure via a range of techniques.Among these,synchrotron-based X-ray techniques with high flux and brightness play a key role in understanding degradation mechanisms.In this comprehensive review,we summarize recent advancements in degra-dation modes and mechanisms that were revealed by synchrotron X-ray methodologies.Subsequently,an overview of X-ray absorption spectroscopy and X-ray scattering techniques is introduced for charac-terizing failure phenomena at local coordination atomic environment and long-range order crystal struc-ture scale,respectively.At last,we envision the future of exploring material failure mechanism.

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.

Ultrasmall CoS nanoparticles embedded in heteroatom-doped carbon for sodium-ion batteries and mechanism explorations via synchrotron X-ray techniques

Transition metal sulfides have been regarded as promising anode materials for sodium-ion batteries(SIB).However,they face the challenges of poor electronic conductivity and large volume change,which result in capacity fade and low rate capability.In this work,a composite containing ultrasmall CoS(~7 nm)nanoparticles embedded in heteroatom(N,S,and O)-doped carbon was synthesized by an efficient one-step sulfidation process using a Co(Salen)precursor.The ultrasmall CoS nanoparticles are beneficial for mechanical stability and shortening Na-ions diffusion pathways.Furthermore,the N,S,and O-doped defect-rich carbon provides a robust and highly conductive framework enriched with active sites for sodium storage as well as mitigates volume expansion and polysulfide shuttle.As anode for SIB,CoS@HDC exhibits a high initial capacity of 906 mA h g^(-1)at 100 mA g^(-1)and a stable long-term cycling life with over 1000 cycles at 500 mA g^(-1),showing a reversible capacity of 330 mA h g^(-1).Meanwhile,the CoS@HDC anode is proven to maintain its structural integrity and compositional reversibility during cycling.Furthermore,Na-ion full batteries based on the CoS@HDC anode and Na_(3)V_(2)(PO_(4))_(3)cathode demonstrate a stable cycling behavior with a reversible specific capacity of~200 m A h g^(-1)at least for 100 cycles.Moreover,advanced synchrotron operando X-ray diffraction,ex-situ X-ray absorption spectroscopy,and comprehensive electrochemical tests reveal the structural transformation and the Co coordination chemistry evolution of the CoS@HDC during cycling,providing fundamental insights into the sodium storage mechanism.

Stress Measurement with an Improved Hollow Inclusion Technique In Jinchuan Nickel Mine

Borehole overcoring stress measurement with an improved hollow inclusion technique was carried out at 10 points on 3 levels in Jinchuan nickel mine which is situated in north-west of China. Through the measurement, 3-D in situ stress state at the measuring points and distribution characteristics of the stress field in the mine were obtained. The stress state in Jinchuan mine is dominated by the horizontal tectonic stress field. The maximum principal stress is horizontal which is about twice the weight of the overburden and its orientation is approximately vertical to the regional tectonic line. The difference between two horizontal principal stresses is quite large which is an important reason to cause failure of underground excavations.

Techniques for in-situ stress measurement at great depth

Reliable information of in--situ stress state is necessary for the design andconstruction of most important rock projects. As most rock projects are getting deeper and deeper,traditional techniques of in--situ stress measurement are not very suitable. The current techniquesof in--situ stress measurement and their insufficiency for use at great depth are analyzed. Somebasic ideas of the development of new techniques and the improvement of current techniques for useat great depth are provided.

Liquid Level Measurement in Oil Tanks Based on Double-differential Pressure Technique

The system principle and configuration of the double differential pressure method for measuring oil tank level are presented. The fundamental method and circuit of fiber optic transmission are analyzed .The accuracy and security of level measurement in the oil tanks have been greatly improved.

Corrosion Measurements of Reinforcing Steel by Different Electrochemical Techniques

Electrochemical techniques of the corrosion measurements of reinforcing steeI in concrete have been evaluated. These techniques include half-cell potential measurements, impressed voltage method, impressed current method and potentiostatic polarization technique. The results of corrosion behaviour of the steel in both 5%NaCl and 5%MgSO4 show that each electrochemical technique provides some information about the condition of the steel bar or the corrosivity of the environment being evaluated, yet none provides a complete data regarding the corrosion resistance of reinforcing steel in aggressive media

Measurement of Concentration Distribution of Electrogenerated Etchant Using an Electrochemical Probe Technique

An electrochemical probe measurement system for detecting an electrogenerated etchant in solution is developed.Concentration distribution of electrogenerated etchant bromine as close as 8 micrometer to the surface of macrodisk is studied quantitatively.

Techniques trend analysis of propagating laser beam quality measurement

Different methods of measuring a propagating laser beam quality are summarized.The disadvantages in traditional way in measuring a laser beam quality is analyzed and the insufficiencies of the Shack-Hartmannin method which is commonly using wave front technique at present is pointed out.Finally,the transmission intensity equation based(TIE-based)measuring way in a laser beam quality evaluation and the corresponding advantages are discussed,which is believed to be a deve-l oping trend in laser beam evaluation.

A Newly Developed Non-Destructive Tritium Measurement Technique and Its Application to V-4Cr-4Ti Alloy

A non-destructive and in-situ technique for the measurement of tritium in materials, namely β-ray-induced X-ray spectrometry （BIXS）, has been developed recently. In the present study a V-4Cr-4Ti alloy was pre-heated at 1000℃ for 2 h to form a recrystallization structure before the tritium absorption experiments were conducted. Firstly the hydrogen isotope gas was charazterized by means of a quadrupole mass spectrometer （QMS） and a small-sized ionization chamber. Then hydrogen isotope absorption tests of V-4Cr-4Ti alloy were performed at 400 ℃ and the atomic concentration of hydrogen isotope in V-4Cr-4Ti alloy was estimated as 0.17% with a tritium content of approximately 2.5 ppm. Experimental results indicate that BIXS is a quite useful tool for quantitatively measuring the tritium content and tritium distribution in the surface layers of vanadium alloys and no strong trapping effects of tritium exist in the pre-heated V-4Cr-4Ti alloy.

Ultrasonic Resonator Techniques for Broad-band Spectroscopy and for High-resolution Sound Velocity Measurement of Liquids

This review gives a short introduction into the principles of ultrasonic measurement techniques for liquids, using cavity resonators. Guidelines for the resonator design in broad-band ultrasonic stxctroscopy as well as in high-resolution single-frequncy or narrowband applications are presented. Deviations of the field configuration in real cells frtxn that in an ideal resonator are discussed and relations for the mode spectrum of cavity fields are given. Recent resonator measurement procedures and methods of data evaluation are mentioned briefly. Some examples of measurements show the extended usability of ultrasonic resonator techniques in basic science and in a wide range of applications for rrkaterials characterization, in manufacturing processes, as well as in control routines.

Technique and experiment of active direct gas pressure measurement in coal roadway

An active measurement method and its principle was introduced consideringthe low success rate,special difficulty,and long measurement time of the direct gas pressuremeasurement currently used in coal roadways.The technology of drilling,boreholesealing depth,borehole sealing length,sealing control of the measuring process,compensatorycomputation of gas loss quantity and other key techniques were discussed.Finally,based on the latest instrument the authors developed,a series of experiments of directgas pressure measurement in the coal roadways of the Jincheng and Tongchuanmine district,were carried out.The experimental results show that active gas pressuremeasurement technique has advantages as follows:(1) the application scope of direct gaspressure measurement technique is wide and it does not have the restriction of coalhardness,coal seam fissure and other conditions;(2) the measured results are credible,which can be tested by the same gas pressure value acquired from a different borehole inthe same place;(3) the measurement process is convenient and quick,it takes about 2 to3 days to acquire the gas pressure value in a coal seam.

Atmospheric NO_2 Concentration Measurements Using Differential Absorption Lidar Technique

Using the Differential Absorption Lidar (DIAL) technique, two types of approaches, namely, reflection from retroreflector / topographic target and backscatter from atmosphere, are available for studying remotely the atmospheric NO, concentration. The Argon ion lidar system at the Indian Institute of Tropical Meteorology (IITM), Pune, India has been used for the measurements by following both the path-averaged and range-resolved approaches. For the former, a topographic target (hill) is used for determining path-averaged surface concentration. In the latter, spectral properties of atmospheric attenuation is used for making range-resolved measurements in the surface layer. The results of the observations collected by following both approaches are presented. The average surface NO2 concentration was found to vary between 0.01 and 0.105 ppm and the range-resolved measurements exhibited higher values suggesting treatment of the lidar data for scattering and extinction effects due to atmospheric aerosols and air molecules, and atmospheric turbulence. Certain modifications that are suggested to the experimental set-up, data acquisition and analysis to improve the measurements are briefly described.

Editorial: Advances in Optical Techniques for Mechanical Measurements

Recently, optical techniques have attracted great attention due to their excellent non-destructive, non-contact, high-resolution, and full-field characteristics. Applications can be found in diverse fields such as precision mechanics and manufacturing, aerospace and automotive testing and inspection, materials science, and biomedical engineering. Advances in Optical Techniques for Me- chanical Measurements presents the latest research progresses in several widely used optical techniques with applications in preci- sion mechanical engineering.

Experimental and Numerical Study of the Effect of Surround Protection Technique on the Strain Measurement for Offshore Jacket Platform

For strain measurement on offshore jacket platform in deep water, waterproof of strain foil is always an important issue, especially, due to the high pressure in deep water. The waterproof is difficult in two places, one is between the matrix structure and the protection structure, and another is between the lead wires and the protection structure. The surround protection technique discussed in this paper is conventional and ideal, and can be operative for a long time, up to five years. In this method, a metal case and tube is added on the local position, which increases the local rigidity, but the effect on the measurement of strain is not well studied. In this paper, the effect of the surround protection technique on the strain measurement is studied by using numerical and experimental methods, and the results show that the measurement error is well in the range permitted by engineering practice.

PROGRESS OF ACOUSTIC WAVE TECHNIQUE ANDITS APPLICATION IN UNDERGROUND PRESSURE MEASUREMENT

This paper carries out tbe experirnent study on the correlation between am stress-strain process of rock samples and the acoustie parameter change of rock by using the measurement system of KS acoustic wave data processing device. On the spot, the stability of surrounding rock is studied by means of experiments on the relationship between the change process (from elastie to plastic failure zone) in surrounding rock of roadway and the change law of acoustic parameters of rock. These acoustie parameters inelude wave amplitude, spectral amplitude, spectrum area, spectral density,wave veloeity and attenuation coefficient etc.

STUDY ON TESTING TECHNIQUE FOR MEASUREMENT OF FATIGUE－CREEP INTERACTION RESISTANCE

By using dropped stress creep method a new testing technique for measurement of the fa-tigue-creep interaction resistance is developed. At varied adjusted mean stresses the creep testingwas performed repeatedly When an unlimited extensive incubation period with zero creep rate oc-curred. the stress cavsing zero creep rate is defined as fatigue-creep resistance. The developped test-ing technique was used to measure the fatigue-creep resistance in F anc C regions. The dynamic ef-fective stress could yield a better descrption of fatigue and creep interaction. The fatigue-creep rateequations with varied exponents inF of C region are established. The different deformation mecha-nisms in F or C regions are indicated

The Relationship between Interchangeability Standards and Precision Design in Teaching a Course on Interchangeability and Measurement Techniques

This article discusses some views on the relationship between carrying out and applying standards and precision design and the teaching of a course on interchangeability and measurement techniques. It points out that while emphasizing precision design, we should not underrate the significance of interchangeability and standardization. Although there are presently many teaching models available for such courses, each course should be designed separately to preserve its systematic character and integrality. As well, the development of students' abilities in precision design and the application of standards should be strengthened in experimental lessons within each course.

Research on Measure Techniques Using CAD-Vector Method for Heteromorphism Leaf Area of Garden Trees

Heteromorphism leaf area of garden trees was measured by CAD-vector method.It was showed that all the coefficients of variation were below 1% when measurement accuracy was relatively high.This method was fit for accuracy area measurement of abnormity leaf,pests and disease leaf,big leaf,small leaf and so on.

The application of synchrotron X-ray techniques to the study ofrechargeable batteries

The increased use of rechargeable batteries in portable electronic devices and the continuous develop-ment of novel applications （e.g. transportation and large scale energy storage）, have raised a strong de-mand for high performance batteries with increased energy density, cycle and calendar life, safety andlower costs. This triggers significant efforts to reveal the fundamental mechanism determining batteryperformance with the use of advanced analytical techniques. However, the inherently complex character-istics of battery systems make the mechanism analysis sophisticated and difficult. Synchrotron radiationis an advanced collimated light source with high intensity and tunable energies. It has particular ad-vantages in electronic structure and geometric structure （both the short-range and long-range structure）analysis of materials on different length and time scales. In the past decades, synchrotron X-ray tech-niques have been widely used to understand the fundamental mechanism and guide the technologicaloptimization of batteries. In particular, in situ and operando techniques with high spatial and temporalresolution, enable the nondestructive, real time dynamic investigation of the electrochemical reaction,and lead to significant deep insights into the battery operation mechanism. This review gives a brief introduction of the application of synchrotron X-ray techniques to the inves-tigation of battery systems. The five widely implicated techniques, including X-ray diffraction （XRD）, PairDistribution Function （PDF）, Hard and Soft X-ray absorption spectroscopy （XAS） and X-ray photoelectronspectroscopy （XPS） will be reviewed, with the emphasis on their in situ studies of battery systems during cycling.