Changes In Structure Of Material Research Articles

Experimental Investigation of Porous and Mechanical Characteristics of Single-Crack Rock-like Material under Freeze-Thaw Weathering

Freeze-thaw weathering changes the pore structure, permeability, and groundwater transportation of rock material. Meanwhile, the change in rock material structure deduced by frost heaving deteriorates mechanical properties of rock material, leading to instability and insecurity of mine slopes in cold regions. In this paper, rock-like specimens containing prefabricated cracks at different angles and having undergone various freeze-thaw cycles are used as the object. Their pore structure, compressive mechanical properties, strain energies, failure characteristics, and the connection between pore structure and mechanical properties are analyzed. Results show that the porosity, spectrum area of mesopores, and spectrum area of macropores increase with the increase in freeze-thaw cycles, while crack angle shows no obvious influence on pore structure. Peak stress and elastic modulus drop with the increase in freeze-thaw cycles, while peak strain shows an increasing trend. Peak stress and elastic modulus decrease in the beginning, and then increase with the increase in crack angle, while peak strain shows a reverse trend. Elastic strain energy and pre-peak strain energy drop with the increase in freeze-thaw cycles. Elastic strain energy decreases first, and then increases with the increase in crack angle. The correlation between the spectrum area of macropores and elastic modulus is the strongest among different pores. Elastic modulus and peak stress decrease with the increase in macropore spectrum area, and peak strain increases with the increase in macropore spectrum area.

Preparation of single-crystal diamond for Small Angle X-ray Scattering in situ loading test

A 2.45 GHz/6 kW cylindrical cavity type microwave plasma chemical vapor deposition reactor was used for the growth of high optical quality single-crystal diamonds. The effects of growth temperature on the surface morphology and crystal quality and the optical properties of the synthesized diamond were studied using optical microscopy, XRD rocking curve, Raman spectroscopy, photoluminescence spectroscopy, Small Angle X-ray Scattering and X-ray topography. Diamond single crystal of the size of Φ7 × 0.5 mm3 were obtained at 1000 °C in a pocket holder with the average growth rate of 7.5 um/h. X-ray rocking curve of the sample was 32 arcsec, while the X-ray transmittance was over 80%. There were no evident NV defects peak in PL. After high pressure blasting test, the diamond windows prepared at 1000 °C can also withstand the pressure of 27 MPa. All these performances were suitable for the windows which was applied on Small Angle X-ray Scattering in situ loading test. Design of a device for Small Angle X-ray Scattering in situ loading test was demonstrated. The device was convenient for the research of material structural changes under high pressure.

Effect of different attributes of the mimic human lumbar spine biomechanics material structure change by finite element analysis

In this study, we compared stress changes and quantity effect relationships from 3D finite element models of normal and degenerative lumbar segments. We further defined the mechanisms causing alterations in mechanical stability the control of normal and degenerative lumbar segments using traditional Chinese medicine. The characteristics of the stress change and the quantity effect relationships of the three-dimensional finite element model of normal and degenerative lumbar segments were compared. The mechanism(s) leading to changes in mechanical stability and the intervention and balance between normal and degenerative lumbar segments of the traditional Chinese medicine was analyzed. The change trend of stress and strain was compared with the three dimensional finite element model under different motion states of normal lumbar vertebrae. A 3D-FEM of degenerative lumbar segments L4 ~ 5 of the human spine was established to simulate the physiological and pathological changes of the lumbar spine in response to flexion, extension, lateral bending and torsion. The stress changes in the normal and degenerative lumbar vertebrae were assessed through external force interventions and the response to TCM. Stress in the degenerative lumbar vertebrae changed according the external load. Stress and strain were compared in the FEM model under a range of motion states. Components of the human lumbar vertebrae including the cortical vertebrae, cancellous bone, endplates, fibrous rings, and facet articular processes were investigated. The elastic modulus of the nerve roots and the posterior marginal structures of the vertebral body increased with lumbar degeneration. Under stress trends in normal lumbar and different degrees of degenerative lumbar structures including cortical bone, loose bone, terminal plate, fiber ring, nucleus, small articular processes, nerve roots and posterior structures. In normal lumbar spine, 20%, 50%, 70% lumbar degeneration, 106 different lumbar anterior flexion 30 and posterior extension with different external forces showed that ANOVA F was between 3.623 and 11.381 and P changed between 0.001 and 0.05.It is clear that in the lumbar movement segments under different pressure intervention, the changes in the degree of degeneration are significantly different from each constituent structure, among which the trend of expected change between the constituent structures of the lumbar anterior flexion 30 is particularly obvious. The stress distribution in the intervertebral discs were influenced by TCM, and the space in the spinal canal enlarged so that nerve root stress decreased, vertebral body stress increased, and facet processes and pedicle stress in the posterior regions exceeded those of the anterior flexion position. The internal stress of the intervertebral disc increased in the flexion compared to the extension position, gradually increasing from top to bottom. The stress concentration point of the degenerative lumbar disc is significantly greater than the stress in the normal lumbar disc stress distribution area, and increases with the degree of degeneration. Compared with the load capacity of normal lumbar and mild (15% reduction), moderate (40% reduction) lumbar disc protrusion model in bending, extension, axial rotation, lateral bending, the results found that the load transmission of lumbar disc degeneration model to different degrees has also changed, so its compression stiffness, strain distribution and size are also different. TCM can improve and treat lumbar disc disease through its ability to regulate the mechanical environment of degenerative lumbar vertebrae. Compared to the FEM models of the lumbar vertebrae, lumbar degenerative changes could be assessed in response to alterations in the biomechanical environment. These findings provide a scientific basis for the popularization and application of TCM to prevent and treat spinal degenerative disease.

Thermo-Optical Characterization of Cu- and Zr-Modified TiO2 Photocatalysts by Beam Deflection Spectrometry

Cu/Zr-modified TiO2 photocatalysts were prepared in the form of nanopowders and characterized by photothermal spectrometry, UV–Vis spectrophotometry and X-ray diffraction (XRD) to investigate the effect of Cu/Zr content on their thermo-optical and transport properties. Adding Cu (0.05%) caused a change in the light absorption range limit, which reduced from 3.25 eV for pure TiO2 to 2.85 eV for Cu-modified TiO2. The decrease in energy band gap was accompanied by a 19.5% decrease in the charge carrier lifetime, which is not favorable for photocatalysis. The decrease in charge carrier lifetime can be minimized by additional modification of TiO2 with Zr (1%), which showed insignificant effects on the energy band gap of the investigated materials. Furthermore, modification of TiO2 with Zr affected the material’s structure and increased its specific surface area, which improved the adsorption of degraded compounds as well as the absorption of light. Altogether, these effects resulted in higher photocatalytic degradation rate constants of the investigated TiO2-based photocatalyst. It was also found that modification of TiO2 with Cu and/or Zr increases both the material’s thermal diffusivity and conductivity due to changes in the band gap and structure of material. Beam deflection spectrometry (BDS) has demonstrated high potential in materials’ characterization which stems from its high sensitivity and precision.

Multilayer MoTe2 Field‐Effect Transistor at High Temperatures

AbstractFunctional 2D material‐based devices are likely subjected to high ambient temperatures when integrated into miniaturized circuits for practical applications, which may induce irreversible structural changes in materials and impact the device performance. However, majority of 2D devices’ studies focus on room temperature or low‐temperature operation conditions. Here, the high‐temperature (up to 673 K) electro‐thermal response of molybdenum ditelluride (MoTe2)‐based field‐effect transistors is investigated. The optimal annealing temperature of around 500–525 K for the multilayer MoTe2 devices with two‐fold enhancement in maximum current level, field‐effect mobility, and current on‐off ratio is identified. Furthermore, MoTe2 devices show the transition of electrical response from gate modulation to the degenerately p‐doped (hole dominant) characteristics when the operation temperature increases to ≈600 K. The gate‐dependent electro‐thermal measurements complemented by surface chemistry analysis confirm the near range hopping transport in the MoTe2 channel at high temperature induced by thermally triggered oxidation of MoTe2. These results not only provide the thermal endurance limits of MoTe2 for practical applications, but also indicate the possible applications of MoTe2 for thermal sensing applications.

Effect of Time-Real Marine Environment Exposure on the Mechanical Behavior of FRP Composites

Fiber reinforced polymer (FRP) composites coupons were exposed to real sea environment to assess the influence on the mechanical behavior of composite materials used in the construction of marine structures. Real-life sea environment conditions were opted for instead of the more common simulated and laboratory versions of seawater in the attempt to obtain more realistic structural modeling environmental input design parameters for marine structures. Exposure was performed over prolonged time span instead of the usual accelerated tests. Epoxy and polyester resins, reinforced with glass fibers in three fiber layout configurations, were used to manufacture standardized tensile testing coupons. Mass changes due to seawater absorption, microorganism growth, changes in tensile strength (standard tensile tests), and surface morphology of the coupons were evaluated after 6- and 12-month long periods of submersion in the sea in the Rijeka bay, Croatia. All specimens showed mass increase due to water absorption and growth of attached algae and sea microorganisms. Various levels of reduction in tensile strength, depending on the fiber layout configurations, were observed. Significant changes in the matrix material structure were noticed, effectively producing “voids”. Based on these results, sustainability of FRP composites in marine environment is addressed and discussed.

Design of an ultrafast electron diffractometer with multiple operation modes* *Project supported by the Director Fund of WNLO (Grant No. WNLOZZYJ1501), the Fundamental Research Funds for the Central Universities, HUST (Grant No. 2017KFXKJC001), the Innovation Fund of WNLO, and the Fund of State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics (Grant No. T152012).

Directly resolving structural changes in material on the atomic scales of time and space is desired in studies of many disciplines. Ultrafast electron diffraction (UED), which combines the temporal resolution of femtosecond-pulse laser and the spatial sensitivity of electron diffraction, is an advancing methodology serving such a goal. Here we present the design of a UED apparatus with multiple operation modes for observation of collective atomic motions in solid material of various morphologies. This multi-mode UED employs a pulsed electron beam with propagation trajectory of parallel and convergent incidences, and diffraction configurations of transmission and reflection, as well utilities of preparation and characterization of cleaned surface and adsorbates. We recorded the process of electron–phonon coupling in single crystal molybdenum ditelluride following excitation of femtosecond laser pulses, and diffraction patterns of polycrystalline graphite thin film under different settings of electron optics, to demonstrate the temporal characteristics and tunable probe spot of the built UED apparatus, respectively.

Limitations of Structural Insight into Ultrafast Melting of Solid Materials with X-ray Diffraction Imaging

In this work, we analyze the application of X-ray diffraction imaging techniques to follow ultrafast structural transitions in solid materials using the example of an X-ray pump–X-ray probe experiment with a single-crystal silicon performed at a Linac Coherent Light Source. Due to the spatially non-uniform profile of the X-ray beam, the diffractive signal recorded in this experiment included contributions from crystal parts experiencing different fluences from the peak fluence down to zero. With our theoretical model, we could identify specific processes contributing to the silicon melting in those crystal regions, i.e., the non-thermal and thermal melting whose occurrences depended on the locally absorbed X-ray doses. We then constructed the total volume-integrated signal by summing up the coherent signal contributions (amplitudes) from the various crystal regions and found that this significantly differed from the signals obtained for a few selected uniform fluence values, including the peak fluence. This shows that the diffraction imaging signal obtained for a structurally damaged material after an impact of a non-uniform X-ray pump pulse cannot be always interpreted as the material’s response to a pulse of a specific (e.g., peak) fluence as it is sometimes believed. This observation has to be taken into account in planning and interpreting future experiments investigating structural changes in materials with X-ray diffraction imaging.

On the transition of reaction pathway during microwave plasma gas‐phase synthesis of graphene nanosheets: From amorphous to highly crystalline structure

AbstractFourier‐transform infrared spectroscopy and proton‐transfer‐reaction–mass spectrometry are used in a complementary way to study gas‐phase processes during decomposition of ethanol in a microwave plasma torch. Decomposition products (C, C2 and simple hydrocarbons) reassemble into higher hydrocarbons and graphene nuclei and further grow into graphene nanosheets (GNS). Depending on microwave power, ethanol flow rate and molecular gas admixture, the material structure changes from amorphous to crystalline. The presence of C2n + 1H y species was found to be responsible for the formation of defects in the GNS structure. O2 and H2 admixtures change the gas temperature axial profile and consequently modify reaction pathways influencing growth and production rate of GNS. Determination of reaction pathway selectivity enables us to predict whether high‐quality or defective GNS are produced.

Manganese Migration in Li1-xMn2O4 Cathode Materials

LiMn2O4 has been considered one of the most promising cathode materials for Li-ion batteries due to its thermal stability, abundance, environmental affinity, and the possibility to exchange Li-ions in three-dimensions. However, it still suffers from major problems, such as capacity fading and voltage decay, which has been associated to phase transformations and dissolution of transition metals. In this report, we use scanning transmission electron microscopy, coupled with differential phase contrast (DPC), to better understand the mechanisms behind the structural transformations occurring in LiMn2O4. We use the fact that DPC has the ability to observe simultaneously light and heavy elements, as well as measure projected electric fields and charge distribution at the atomic level. This approach allows us to monitor the migration of very low amounts of Mn to the Li atomic positions, at the surface and subsurface regions, which otherwise is very challenging to observe using other techniques such as HAADF and ABF. These observations not only provide a fundamental understanding of the structure of LiMn2O4 but also reveal DPC as a novel technique to determine local structural changes in materials consisting of heavy and light elements, as well as identify the location of light elements, monitor low concentrations of substitutional species and identify phase transformations.

In Vitro Study of Octacalcium Phosphate Behavior in Different Model Solutions

Octacalcium phosphate (OCP), a new-generation bone substitute material, is a considered precursor of the biological bone apatite. The two-layered structure of OCP contains the apatitic and hydrated layers and is intensively involved in ion-exchange surface reactions, which results in OCP hydrolysis to hydroxyapatite and adsorption of ions or molecular groups presented in the environment. During various in vitro procedures, such as biomaterial solubility, additive release studies, or the functionalization technique, several model solutions are applied. The composition of the environmental solution affects the degree and rate of OCP hydrolysis, its surface reactivity, and further in vitro and in vivo properties. The performed study was aimed to track the structural changes of OCP-based materials while treating in the most popular model solutions of pH values 7.2–7.4: simulated body fluid (SBF), Dulbecco’s phosphate-buffered saline (DPBS), supersaturated calcification solution (SCS), normal saline (NS), and Dulbecco’s modified Eagle’s medium (DMEM). Various degrees of OCP hydrolysis and/or precipitate formation were achieved through soaking initial OCP granules in the model solutions. Detailed data of X-ray diffraction, Fourier-transform infrared spectroscopy, atomic emission spectrometry with inductively coupled plasma, and scanning electron microscopy are presented. Cultivation of osteosarcoma cells was implemented on OCP pre-treated in DMEM for 1–28 days. It was shown that NS mostly degraded the OCP structure. DPBS slightly changed the OCP structure during the first treatment term, and during further terms, the crystals got thinner and OCP hydrolysis took place. Treatment in SBF and SCS caused the precipitate formation along with OCP hydrolysis, with a larger contribution of SCS solution to precipitation. Pre-treating in DMEM enhanced the cytocompatibility of materials. As a result, on performing the in vitro procedures, careful selection of the contact solution should be made to avoid the changes in materials structure and properties and get adequate results.

T1-T2* relaxation correlation measurements

The majority of low field Magnetic Resonance (MR) analyses rely on T2 lifetime measurements. Modification of the T2 measurement to include a T1 dimension has made the T1-T2 measurement a very powerful analytical technique. The T1-T2 measurement is uniquely well suited to characterization of different spin populations in porous materials, such as fluid bearing reservoir rocks, and in soft biopolymer materials, for example foods. However, the T1-T2 measurement is challenging or impossible if the T2 relaxation lifetime, or a component lifetime, is short-lived and the signal unobservable in an echo measurement. This occurs in many important classes of materials. A short lifetime T2 will not however, in general, preclude observation of a free induction decay with signal decay governed by T2*.As outlined in this paper a T1-T2* measurement is a useful analog to the T1-T2 experiment. T1-T2* measurement enables one to differentiate species as a function of T2* in one dimension and T1 in the other dimension. Monitoring changes of the T1-T2* coordinate, and associated signal intensity changes, has the potential to reveal structural changes in materials evolving in time. These methods may also be employed to discriminate and identify solid-like species present in static samples.The T1-T2* measurement is very general in application, but in this paper we focus on cement-based mortars to develop and illustrate the essential ideas. T1-T2* results show a multi-modal behaviour of the MR signal lifetimes, T1 and T2*, in mortar samples under study, indicating at least two different water populations. The short T2* lifetime was assigned to interlayer water (water between C–S–H layers) where the associated T1 is also short lived. The longer T2* lifetime was assigned to water in the pore space, where T1 is also longer lived. In addition to mortar samples we also show application of the method to a crystalline organic species, o-phenylenediamine, which features Sinc Gaussian and exponential decays of transverse magnetization.

Electrochemically manipulating BiFeO3 particles via Bi3+ ion extraction

AbstractBecause multifunctional ceramics are widely used in the electronics, manipulating composition and structure of the electronic ceramics aim at improving the performance of the target material for appropriate applications. However, the composite materials with multiphases and multicomponents could be achieved by mixing the nanomaterials with various preparing methods or technologies, which generally require a bunch of experimental design to obtain the target products. For achieving the goals, a novel electrochemical approach for preparing functional ceramic materials is demonstrated via ion extraction from the A site of perovskite BiFeO3 (BFO) ceramic particles, and whereby a single‐phase perovskite BFO could be evolved into multiphase and multicrystalline homogeneous composites. With gradual changes in material particle size, composition, structure, and morphology upon electrochemical Bi3+ ion extraction, the magnetic and electromagnetic properties of the decomposed BFO along with the generated multiphase and multicrystalline composites would present pronounced evolutionary behaviors, compared with original BFO. Apparently, such titration method upon electrochemical ion extraction could be employed to manipulate the properties of the functional ceramics. The simple strategy of electrochemical manipulation BFO would be applied to certain materials with electrochemical activity to achieve the target performance.

ИДЕНТИФИКАЦИЯ ИСТОЧНИКОВ АКУСТИЧЕСКОЙ ЭМИССИИ В ПОЛИМЕРНОМ КОМПОЗИЦИОННОМ МАТЕРИАЛЕ В УСЛОВИЯХ ЦИКЛИЧЕСКОГО РАСТЯЖЕНИЯ

The structure of polymer composite materials (PCM) provides high mechanical properties but, at the same time, is highly sensitive to the formation of internal defects. Therefore, when designing, manufacturing products, and assessing their reliability in service, much attention is paid to the methods of non-destructive testing, among which the method of acoustic emission (AE) has proven itself to study structural changes in material under external influence. The paper deals with the identification of typical damages in fiberglass samples made of T11-GVS9 glass fiber cloth and DION 9300 FR binder and tested under cyclic tension using the AE method. In the work, the authors solved the problem of selecting the AE informative parameters and used a clustering method to identify the nature and the formation kinetics of the AE sources. The authors performed clustering using the Kohonen self-organization map (SOM) with the Fourier spectra calculated for the AE signals recorded during cyclic tests. Based on the peak frequencies analysis of the produced clusters, the researchers determined their nature and calculated the periods of critical accumulation. When characterizing the AE sources, the authors used the peak frequencies analysis of the wavelet spectra performed for different levels of decomposition. The authors determined the damage accumulation stages of samples during testing based on own research and research by other authors’ results. The study established that registration of AE signals identified as adhesion failure can be used to identify the onset of the material destruction and characterized the local formation of micro-damages in the matrix and fracture of fibers can be used to predict the destruction of PCM.

Present problems of vibration isolation in heavy mining machines at long-term cyclic loads

Abstract. An integrated approach was used, including the construction of a mathematical model and the results of lengthy industrial tests of heavy mining machines with rubber elastic bonds. The issues of vibration isolation of heavy machines operating in extreme conditions, i.e. with prolonged cyclic loads and the influence of an external aggressive environment inherent in mining and processing enterprises. As an example, we con-sider vortex mixers with a vibration isolation system containing rubber elements. During long-term operation, the mass of the mixer does not remain constant; its increase is associated with the sticking of the initial product on the moving parts of the ma-chine. The location of such machines in the sinter factory at + 10.4 m, as well as the change in time of rotational symmetry of the drum rotation imposes certain requirements on the vibration isolation system: the system must be "soft" and stable in time, i.e. during 9-10 years of operation, its stiffness and dissipative parameters should not go beyond the permissible values. In order to reduce the aging effect, type 2959 rubber based on natural caoutchouc with a reinforced protective group was used, while the instability of the main mechanical parameters was taken into account in the developed theory of vibration isolation of machines. On the basis of the developed simulation model and the Boltzmann-Volterra integral relations with kernels of relaxation and aftereffect, an equation was worked out, which made it possible to take into account the rubber viscoelastic properties in full volume; in this equation, stiffness operator of elastic suspension in the machine is written by using fractional exponential function of the Yu. Rabotnov's type; on the basis of the mathematical model, the basic parameters of the machine under the study were calculated; in particular, for the vortex mixer, the time dependences of amplitude of the mixer housing vibrations and coefficient of vibration isolation efficiency were calculated with taking into account aging of elastic link material in the ma-chines; the calculation results were compared with the results of industrial tests of the vortex mixer operation lasting for 16 years. The theory and method for calculating vibration isolation systems with rubber elastic links for heavy mining machines were developed with taking into account material structure changes due to the effects of aging. The paper considers an example of calculating the mixer vibration isolation system taking into account rubber aging; the magnitude of the change in time of the main mechanical parameters was obtained experimentally over 16 years. This made it possible to determine temporary changes in the amplitude of oscillations of the mixer body and the coefficient of efficiency of the vibration isolation system. It was shown that the mixer vibration isolation system remained effective for 9-10 years, after which the mechanical characteristics of the rubber went beyond the permissible values and the system lost its functional pur-pose, and the amplitude of the mixer body exceeded the existing sanitary standards.

Влияние методов измельчения бересты на выход биологически активных веществ

Introduction. Birch bark contains biologically active substances (BAS). In this regard, the search for ways to increase yield of its bioactive agents is relevant. Aim. To study the effect of birch bark grinding methods on the extract of its BAS during extraction. Materials and methods. Samples of birch bark of silver birch (Betula pendula Roth.) and downy birch (Betula pubescens Ehrh.) were ground up on devices with various force effects on plant material — disk (mainly squeezing, shear, tensile and shearing forces), three-roll annular (crushing and abrasive forces) and ball (crushing, abrasive and shock-shear forces) mills. Morphological and microscopic studies were carried out, the content of extractive substances and moisture in the ground up samples was determined. The composition and content of BAS were analyzed. Results. The smallest changes in the morphological and anatomical structure of plant material were observed when using a disk mill (the morphological features of birch bark and its cellular structure are preserved), grinding on three-roll ring and ball mills leads to serious changes in the morphological and anatomical structure of birch bark (the morphological and anatomical structure is lost, cell walls are destroyed). Comparative analysis of the yield of extractive substances from ground up birch bark samples, depending on the grinding method and the extractant used (purified water and ethyl alcohol of different concentrations: 96, 80, 70, 40, 20 and 10%) showed that the best extractant is 80% ethyl alcohol. The highest yield of extractive substances was noted for a sample of birch bark ground up in a ball mill — 36.85%, for ground up in a disc mill — 29.96%, on a three-roll ring mill — 30.88%. When studying the yield of the main groups of BAS (saponins, tannins, coumarins, hydroxycinnamic acids) from ground up birch bark samples, it was found that when using grinding methods that do not lead to the destruction of cell walls, the yield of BAS is limited by the capillary-porous structure of the plant material. Conclusion. When using grinding methods that lead to the destruction of cell walls, the greatest yield of BAS from birch bark is observed in the case of using a more severe impact on it, including not only abrasion, crushing, but also impact (ball mills).

Metrología óptica en el estudio de eventos dinámicos

The evolution over time of structural changes in materials is of great importance in various areas of science, its study involves determining the phase with the change in the intensity of the physical properties to be measured. In this work, the use of Phase Displacement Interferometry PSI is presented using a combination algorithm of five interferograms or five steps, the results are compared with the addition of the states studied in the dynamic event, exposed in the Digital Holographic Interferometry DHI. The deformation was simulated from a rotating system in the coordinates (x, y). The results suggest that the phase map of the changing events with time that are calculated with PSI of five steps may have a relationship with the average of each change point of the dynamic event, with a difference of 0.96 radians.

Simultaneous Monitoring of Structural Changes and Phase Distribution of LiFePO4 Along the Cathode Thickness of Li Metal Polymer Battery

Probing the structural changes that electrode materials undergo during electrochemical cycling while monitoring their spatial distribution within the volume gives valuable insights on dynamic processes, i.e. side reactions and evolution of phase migration barriers, often associated to capacity and power limitation. In this work, we present an electrochemical cell to perform spatial and time resolved operando synchrotron X-ray diffraction on Lithium (Li) metal polymer batteries operating at 80 °C. A 3.2 mm diameter battery made of a Li metal anode, a LiFePO4 based cathode, and a solid polymer electrolyte acting as separator, is placed inside a glass-based casing and cycled at a beamline. The cylindrical cell geometry with its small size enables to follow the phase transformations occurring at different states of charge and at different cathode heights. It is possible to create spatially resolved phase distribution plots and to differentiate active material structural changes occurring close to the interface with the electrolyte from those at the current collector vicinity. The results provide a direct observation of the Li diffusion in the LiFePO4 and FePO4 phase distribution. In addition, synchrotron X-ray diffraction computed tomography (XRD-CT) measurements were performed to obtain phase distribution maps at different heights of the battery assembly.

Preparation and Characterization of Potato Starch Copolymers with a High Natural Polymer Content for the Removal of Cu(II) and Fe(III) from Solutions.

Cross-linked potato starch (StMBA) and starch-g-polyacrylamide materials with a high content of natural polymer from 60 to 90 wt.% (St60–St90) were synthesized by double chemical-chemical modification (grafting and cross-linking). Eco-friendly starch absorbents were tested for removal of Cu2+ and Fe3+ from aqueous solutions. The characteristics of the obtained materials (Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), thermal analysis (TGA), X-Ray Diffraction (XRD) and laser scanning microscopy (LSM)) confirmed their diversity in terms of composition and structure. The effect of N,N’-Methylenebisacrylamide (MBA) and polyacrylamide (PAM) content in the starch graft copolymers, treatment time and concentration of metal ions on adsorption efficiency were investigated. The adsorption efficiency for StMBA was 14.0 mg Cu2+/g and 2.9 mg Fe3+/g, regardless of the initial concentration of ions, whereas for starch graft copolymer St60 it was 23.0 mg Cu2+/g and 21.2 mg Fe3+/g. Absorption of Fe(III) was persisted even after 2 days. Pseudo-second order model was used to investigate the adsorption mechanisms. It was found that in addition to the chemical adsorption of ions on the surface, there is sorption inside the polymer network and chelating mechanism may dominate. Satisfactory results were attributed to the adequate grafting of PAM onto starch, the ability to form complexes with metal cations and changes in material structure.

The Role of Deformation Bands in Dictating Poromechanical Properties of Unconsolidated Sand and Sandstone

AbstractCataclastic shear bands in sands and sandstones are typically stronger, stiffer, and exhibit lower permeability than the surrounding matrix, and therefore act as barriers to fluid flow. Previous work has quantified the reduction in permeability associated with these features; however, little is known about the role of shear band structure in controlling the way they impact permeability and elastic properties. Here, we report on a suite of laboratory measurements designed to measure the poromechanical properties for host material and natural shear bands, over effective stresses from 1–65 MPa. In order to investigate the role of host material properties in controlling poromechanical evolution with stress, we sampled shear bands from two well‐studied sandstones representing structurally distinct end‐members: a poorly cemented marine terrace sand from the footwall of the McKinleyville thrust fault in Humboldt County, California, and a strongly‐cemented sandstone from the hanging wall of the Moab Fault in Moab, Utah. The permeability‐porosity trends are similar for all samples, with permeability decreasing systematically with increasing effective stress and decreasing porosity. The permeability of the host material is consistently >1 order of magnitude greater than the shear bands for both localities. For the unconsolidated case, shear bands are less permeable and stiffer than the host material, whereas for the consolidated case, shear bands are slightly less permeable, and wave speeds are slower than in the host. We attribute the differences between the McKinleyville and Moab examples to changes in structure of the nearby host material that accompanied formation of the shear band.