True Particle Size Research Articles

Investigation of flocculation behavior of tailings during settling-concentration: influence of true density, particle size, and mud layer height

The rapid concentration of tailings is a crucial initial step in the cemented paste backfill (CPB) process, as it ensures the stability of the backfilling slurry concentration and the continuity of the backfilling process. The structure of flocs plays a pivotal role in tailings concentration, directly contributing to such critical technical parameters as settling speed and bottom flow concentration. However, most of the current studies focus on flocculant addition rather than the tailings slurry itself. Also, there is a lack of uniform characterization of the flocculant structure in the flocculation and settling system. This study establishes a semi-quantitative assessment system for evaluating the fine structure of tailings flocs based on indicators such as the exposure state of coarse particles, floc size, and floc compactness (porosity). The findings reveal that, during the settling process, the higher true density of tailings (3.156 g/cm3) and intermediate particles (40 wt% of 38 μm–74 μm particles) attenuates the clamping effect of turbulence on settling, leading to a faster settling rate to 0.65 cm/s and 0.29 cm/s respectively. Moreover, in the thickening process, tailings located at the bottom of the mud layer expedite the precipitation of interstitial water within the floc structure through the combined influence of gravity and rake frame shear. Consequently, a denser floc structure forms, as evidenced by a higher concentration of bottom flow at a macroscopic level. This conclusion provides a theoretical basis for faster preparation of highly concentrated tailings slurry in CPB.

Valorization of Kraft Pulp and Paper Mill Slaker Grits and Biomass Fly Ash as Fillers in a Commercial Screed Mortar Formulation.

Slaker grits (SG) and biomass fly ash (BFA), two waste streams generated in the pulp and paper industry, are commonly disposed of in landfills, a practice with a high economic and environmental burden. In this work, their individual valorization as fillers in a commercial screed mortar formulation was evaluated in order to achieve a more sustainable management practice. The waste streams were characterized in terms of true density, particle size and morphology, and chemical and mineralogical composition. The influence of their incorporation amount (5.0, 7.5, and 10.0 wt.% of the total solids) and pre-treatment (sieving and grinding) on the fresh (workability) and hardened state (density, water absorption by capillarity, and flexural and compressive strength) properties of the mortars were assessed. The results show that the addition of 10.0 wt.% of the SG after milling and sieving (<75 µm) and 7.5 wt.% of BFA in the as-received condition, or up to 10.0 wt.% after grinding and sieving (<63 µm), allowed for the production of mortar samples with properties within the recommended specifications and that were resistant to 25 consecutive freeze-thaw cycles. This waste valorization route could represent an economic benefit of up to 8.85 €/tmortar and 2.87 €/tmortar for mortar, and pulp and paper companies, respectively.

Influence of a batch of hollow glass microspheres with different strength grades on the compression strength of syntactic foam

Nowadays, syntactic foam filled with hollow glass microspheres (HGM) has been widely used in aeronautical and marine structural applications. In order to obtain a lightweight and high strength syntactic foam, a batch of HGM is usually filled into a resin matrix at a high-volume percentage. Therefore, the strength of syntactic foam was largely dependent on the strength of HGM. In general, a batch of HGM is usually composed of many individual glass microspheres with different true densities, particle sizes, and wall thicknesses, result in differences of the strength, which may lead to the difference in failure mechanism of syntactic foam. However, the strength distribution of a batch of HGM and its influence on the compression strength of syntactic foam has rarely been studied. In this work, the T30-P HGM were obtained by a batch of T30 HGM under five grades isostatic pressure P (P = 10, 20, 30, 40, 50 MPa) treated then floatation. Afterwards, the T30-P HGM were respectively incorporated into epoxy resin E51 with volume fraction of 70% to fabricate syntactic foams SF-T30-P. The results indicated that the compression strength of the syntactic foams was improved from 35.3 MPa to 49.8 MPa nonlinearly with the increasing strength of T30-P HGM. The failure mechanism of the syntactic foams was analyzed and the recommendations for preparing syntactic foams with optimal strength were proposed.

Experimental investigation of a light extinction based sensor assessing particle size and distribution in an oil system

Optical particle counters (OPCs) based on the light extinction measurement scheme are widely used in the industry for monitoring the level of wear debris in lubricating oil systems. In this work it is investigated how model-based size estimation and OPC output data can be correlated. Spherical metal coated 5–20 μm diameter particles were used in a laboratory oil system and monitored using an OPC. The raw OPC output data were extracted with the purpose of estimating the true particle size. Distribution parameters has been deducted from detected minima in output signals for each particle diameter using a half-normal fit centered at the detected kernel peak. Experiments with different sized particles showed that signal minima amplitude distributions differ between particle diameters thus, clearly showing the discrimination ability of the OPC. Furthermore, to obtain OPC based true size determination, the apparent absorption coefficient of the micrometer sized particles must be considered. Thus, reducing the maximum deviation between true and OPC determined diameter to 13%.

Effect of particle size and dust layer size on ignition characteristics of PMMA dust layer on hot surface

Deposition of combustible dust on a hot surface is a hidden danger of fire. In this work, polymethylmethacrylate (PMMA) dust was selected to analyse the influence of dust layer diameter, dust particle size and dust layer thickness on the ignition characteristics of PMMA dust layer. Critical heating temperatures and ignition time had been measured. The STA-GC/MS-FTIR analysis was used to determine that the main products of PMMA pyrolysis were MMA, CO, CO2, and C2H4, of which CO and C2H4 were transported to the ambient to cause gas phase combustion on the surface of the dust layer. For 10 mm thick dust layer, the critical heating temperatures of 5 μm PMMA, 100 nm PMMA, and 30 μm PMMA were 300 °C, 330 °C, and 320 °C. As the thickness of the dust layer increased, the gas transport path became longer, the critical heating temperature and ignition time increased. The characteristic particle size (D [3,2]) was utilized to represent the true particle size, and the ignition time increased with the increase of the characteristic particle size. The increase in the diameter of the dust layer had a slight effect on the temperature history and ignition time of the dust layer.

Iron removal stations’ sludges postprocessing for its resource potential identification

Introduction. The sludge of the washing waters of the underground water iron removal station is a large-tonnage technogenic waste that is dangerous for the environment. The homogeneous chemical composition and finely dispersed structure of the sludge make it possible to consider it as a valuable raw material for the production of various products in the conditions of a forward movement towards a circular economy. Obtaining nanosized metal powders from the sludge of iron removal stations has a number of advantages over traditional physical, chemical and mechanical methods. To optimize the process of obtaining highly dispersed metal powders from the sludge of iron removal stations, it is necessary to study the influence of the main technological parameters on the size, shape and chemical composition of the final material.&#x0D; Materials and methods. Thermal treatment of the sludge of the iron removal station in the carbon monoxide medium was carried out in the temperature range of 400–600 °C. Ultrasonic dispersion was used to get an idea of the true particle size. The granulometric composition of the sludge was studied by electron microscopy and laser beam scattering.&#x0D; Results. The results of experimental studies of the granulometric composition of the treated sludge of iron removal stations are presented. The particles obtained at a temperature of 450 °C had the most pronounced spherical shape, low open porosity, and a low degree of adhesion to neighboring particles. These properties are key for micro- and nanopowder-based products. An increase in the temperature of sludge processing led to the adhesion of particles and their fusion into large aggregates with a brittle structure as a result of the development of crystallization processes.&#x0D; Conclusions. The proposed methods of physicochemical treatment in an environment of carbon monoxide and ultrasonic action of the sludge of an iron removal station, which is currently a technogenic waste, makes it possible to obtain a highly dispersed metal powder. This material has the necessary properties for use in modern high-tech industries.

Oxidative removal of soluble divalent manganese ion by chlorine in the presence of superfine powdered activated carbon

Here, we examined the removal of soluble divalent manganese (Mn(II)) by combination treatment with superfine powdered activated carbon (SPAC) and free chlorine in a membrane filtration pilot plant and batch experiments. Removal rates >95% were obtained with 3 mg/L SPAC, 1 mg/L chlorine, and a contact time of 4 min, meeting practical performance standards. Mn(II) was found to be oxidized and precipitated on the surface of the activated carbon particles by chlorine. The Mn(II) removal rate was fitted to pseudo-first-order reaction kinetics, and the rate coefficient changed in inverse proportion to as-is particle size, but not to true particle size. The rate coefficient was independent of both Mn(II) concentration, except at high Mn(II) concentration, and the chlorine concentrations tested. The rate-determining step of Mn(II) removal was confirmed to be external-film mass transfer, not chemical oxidation. Activated carbon was found to have a catalytic effect on the oxidation of Mn(II), but the effect was minimal for conventionally sized activated carbon. However, Mn(II) removal at feasible rates for practical application can be expected when the activated carbon particle diameter is reduced to several micrometers. Activated carbon with a particle size of around 1–2 μm may be the most appropriate for Mn(II) removal because particles below this size were aggregated, resulting in reduced removal efficiency.

Scaled-up rice grain modelling for DEM calibration and the validation of hopper flow

Industrial-scale simulation of the interaction between rice grains and equipment using the discrete element method (DEM) is limited due to the high computing power requirement. Volume-based scaled-up modelling of DEM rice particle and calibration of DEM input parameters were investigated as an alternative approach towards realising industry scale simulation-based design support of rice grains flow behaviour. Calibration of DEM input parameters using scaled-up DEM particles is challenging because distortions in the DEM material properties due to unavoidable disparities between the true and DEM particle sizes. A DEM calibration methodology that applies virtual design of experiment (DOE) using scaled-up DEM rice particle model was applied to predict bulk angle of repose (AOR) of unshelled rice grains. Rice DEM particle shape was scaled-up by three times its original prolate spheroid particle shape and then approximated using seven-clumped DEM spheres matching the scaled-up spheroid rice particle. Using DEM parameter values of the rice model calibrated to match AOR at a relative error (RE) of 0.39%, the DEM model predicted hopper discharge rates from experiment and using the analytical solution of Beverloo et al analytical solution at relative errors (REs) of 0.66% and 0.03%, respectively. Hopper unloading time predicted by DEM had a RE of 0.93% when compared with experiment. A 60% saving in CPU time was achieved relative to the unscaled DEM rice particle model with good agreement to the rice flow test. This showed that the techniques of volume-based particle scaling and DOE calibration are effective methods for industry-scale simulation of small grains.

Effects of particle size on two-phase flow loss in aluminized solid rocket motors

This study investigates the two-phase flow loss in aluminized solid rocket motor (SRM) by addressing the effects of particle size. A simplified axisymmetric 2D numerical simulation model is developed to simulate the flow field of the SRM, in which the two-phase flow consists of seeded inert Al2O3 particles and burned gas. The numerical model is verified by lab-scale SRM tests. The results show that the numerical simulation predicts SRM performance accurately when quantitatively capture the true particle size. Based on numerical simulations over a broad range of particle diameters, the effects of particle size on the gaseous phase and particle velocity distributions, particulate trajectories, and the thrust coefficient are systematically examined. It is found that with the same mass content of inert particles the two-phase flow loss decreases with increasing particle size.

Measuring bulk density variations in a moving powder bed via terahertz in-line sensing

Monitoring the relative density of static or moving powder inside a process line is essential for manufacturing high-quality products. The aim of this study was to predict density variations in a moving powder bed using terahertz reflection technology. We systematically investigated three grades (varying true density and particle size) of two materials: lactose and silicified microcrystalline cellulose (SMCC). These six powders specifically differ in their compressibility, which can be applied to assess the sensitivity and applicability of our method. The powders were filled into a round container, and terahertz reflection measurements were acquired continuously during the container’s rotation. The setup allowed to adjust the relative density by compacting the powders into specific powder bed heights. Each powder was compacted to various relative densities (compression pressures up to 100 kPa). We calculated the surface refractive index based on the in-line terahertz measurements acquired during rotation, which has a linear dependence on the relative density of the powder. This was confirmed by correlating the refractive index values with the theoretical relative densities based on the bulk and true densities of the powder. The coefficient of determination (R2) was larger than 0.962 (Lactohale 100) for all six powders, with the highest coefficients for Lactohale 220 (R2 = 0.996) and SMCC 50 LD (R2 = 0.995). The results suggest that the proposed method can resolve relative densities averaged across the powder bed that are as small as 0.3% (Lactohale 100). The high acquisition rate of the terahertz system (15 Hz) made it possible to determine the powder density in 230 positions uniformly distributed throughout the container, facilitating the investigation of the relative density uniformity in the container as a function of the powder bed height. It was observed that SMCC powders undergo a smaller change in the relative density variations upon compaction than the lactose powders. Moreover, the relative density maps clearly indicate local density differences in the powder bed for all powders. The relative density variations that were introduced by packing of the container prevailed throughout the compaction process for all samples with the exception of Lactohale 220. The presented approach allows a precise resolution of the spatial distribution of relative density, which facilitates an in-depth analysis of powder behavior upon compaction.

A rheometry based calibration of a first-order DEM model to generate virtual avatars of metal Additive Manufacturing (AM) powders

The technology of metal powder-bed Additive Manufacturing (AM) has been evolving rapidly over the last few years. Creating parts through additive manufacturing within acceptable tolerances for porosity, strength and roughness is contingent upon many process variables. One important factor is the ability to spread uniform layers of loose powder for a given thickness over a given coverage area. This is related to the angle of repose of the powder and its rheological behavior i.e., the flow or shear motion of the powder. As in the case of spreading which is essentially a shear flow under a load, in this work, a benchtop powder rheometer with the capabilities to study bulk flow performance of AM powders is utilized to characterize a metal AM powder. When used in tandem with powder dynamics modeling, the rheometer can provide the powder rheological parameters to quantify ‘spreadability’ i.e., the ease with which a powder will spread under a specified set of conditions. Powder dynamics modeling using the discrete element method (DEM) can simulate powder spreading and capture powder layer quality descriptions such as segregation, porosity and surface roughness but needs to account for true particle shapes and sizes. The requirement to simulate realistic particle shapes and sizes results in computationally expensive DEM simulations with millions of particles. This study is therefore directed towards modeling bulk powder performance and determining the minimum volume of powder to be simulated to understand its rheological properties. This work aims to calibrate a virtual media with monodispersed spherical particles against angle of repose and rheological properties of a real media made up of almost spherical particles and comparable sizes. This calibrated media, which is the “virtual avatar” of the real powder, is also tested for rheological properties at varying load conditions and can further be made available to study the ‘spreadability’ of AM powders. The model compares well with published results for a benchmark granular media (2 mm glass beads) and has moderate accuracy for in-house experiments on a well-known AM powder (100 − 250μm Ti-6Al-4V). CPU-based serial computing is used for modeling around 8000 2 mm glass beads and subsequently, significantly faster GPU-based parallel computing is used to model 1.3 million 250μm Ti-6Al-4V powder.

Assessing the benefits of automatic grinding control using PST technology for true on-line Particle Size Measurement

Despite the recognized significance of ground product fineness on both line capacity and downstream process performance (typically flotation), less than 10% of mineral ore concentrators today use real-time particle size measurements in automatic control applications for the final product particle size. Although “near-line” particle size measurement instrumentation has been in place for several decades and is commonly installed in most modern concentrators, its availability and low measurement frequency have typically been inadequate for reliable use in automatic control. Their low availability is often associated with problems with slurry sample collection and handling systems required to present the samples to the size measurement instrument. Recently, an innovative technology for real-time, on-line particle size measurement has been developed by CiDRA Minerals Processing, under its commercial name Particle Size Tracking (PST), already proven in several commercial installations, demonstrating near 100% availability with minimal maintenance, thus overcoming the limitations of previous technologies. Investment decision makers require convincing, reliable estimates of the expected economic value that automatic grind control projects will deliver. This paper presents a methodology for estimating such value from the installation of the new PST particle size measurement technology, capable of tracking particle size on each individual hydrocyclone overflow stream, thus adding significant new options for improved process stability and performance. Based on actual plant operating records, accumulated over long periods of time, the evaluation approach herein described assesses and highlights the significant potential contribution to be expected from this unique PST technology.

Methodology for assessing the benefits of grind control using particle size tracking technology for true on-line particle size measurement

Methodology for assessing the benefits of grind control using particle size tracking technology for true on-line particle size measurement

Microstructural Characterization of Ni/YSZ Electrodes in a Solid Oxide Electrolysis Stack Tested for 9000 Hours

The performance of solid oxide electrolysis cells (SOEC) is affected by microstructural changes inside the cell. In this work detailed post-mortem characterization is conducted on an SOEC stack tested for electrolysis of steam over 9000 h [1]. The stack, produced by Topsoe Fuel Cell A/S, consists of 25 identical repeating units connected in serial. Each repeating unit includes an SOEC cell and neighboring interconnects (ICs). The SOEC cell has a Ni-YSZ support layer and fuel electrode, a YSZ electrolyte, a LSCF-CGO (LSCF: (La,Sr)(Co,Fe)O3-δ, CGO:(Ce,Gd)O2) oxygen electrode and a CGO barrier layer between the electrolyte and the oxygen electrode. The objective of the present investigation is to identify modifications in the active Ni-YSZ electrode microstructure, which are believed to strongly affect the SOEC cell and stack performance. These microstructural changes are quantified thorough 2D and 3D microstructure analyses. Based on micrographs recorded for the 9 kh tested stack and a reference cell (i.e. a cell from the same production batch as those in the stack, but not long-term tested), a relative quantification of Ni, YSZ and pore phase fractions and particle sizes has been obtained through scanning electron microscopy (SEM) imaging analysis. The mean intercept length principle has been used to investigate 2D SEM images recorded on different cell locations. The ease of this type of characterization makes it possible to investigate several locations in the long term tested stack: both fuel electrode inlet and outlet, directly under the contact point between the IC and at the point where the cell is in contact with the gas channel. By comparing results of the reference and tested cell, significant changes in Ni and pore size are observed while the YSZ backbone does not show substantial changes. The 9000 h electrolysis testing results in a decrease in the Ni phase fraction and an increase in Ni particle size. Compared to the reference cell, the biggest microstructural change is observed at the location where the cell is directly in contact with the IC, where the Ni phase fraction is decreased from 28 % (reference) to 18 % and the Ni mean intercept length is increased from ~1 μm (reference) to ~1.4 μm. Based on the 2D image analysis locations of special interest were selected for 3D reconstruction of the electrode structure by focused-ion-beam (FIB) serial sectioning. The 3D data provides information on the true particle size distribution, avoiding the assumptions that need to be made for the 2D data. Besides, the 3D analysis allows the transport pathways to be characterized through each of the phase networks [2]. A comparison between 2D and 3D data is carried out to concisely investigated microstructural changes and relate them with the cell performance during long-term operation. [1] A. Brisse, J. Schefold, G. Corre, Q. Fu. Performance and Lifetime of Solid Oxide Electrolyzer Cells and Stacks. 11thEuropean SOFC & SOEC Forum, July 2014 [2] Peter Stanley Jørgensen, Søren Lyng Ebbehøj, and Anne Hauch. "Triple phase boundary specific pathway analysis for quantitative characterization of solid oxide cell electrode microstructure." Journal of Power Sources 279 (2015): 686-693. Figure 1

Assistance for Predicting Deposition of Tranilast Dry Powder in Pulmonary Airways by Computational Fluid Dynamics

Computational fluid dynamics (CFD) simulation was performed to predict deposition behavior of the dry powder inhaler (DPI) formulation in a pulmonary airway model. A synergistic study on CFD simulation and sample preparation with highly branched cyclic dextrin (HBCD) as an excipient matrix for dry powder inhaler formulations of tranilast (TL) were performed. The crystal form of TL in spray-dried particles was characterized by powder X-ray diffraction and fluorescence spectroscopy. The aerodynamic performance of DPI formulations was assessed using the Andersen cascade impactor. CFD simulations could simulate the movement of fluids by resolving the mathematic equations governing the movement following Navier-Stokes equations. Particle behavior and deposition from CFD analysis compared with experimental data. Spray-dried particles (SDPs) of TL/HBCD showed characteristic diffraction peaks differing from untreated TL crystalline in powder X-ray diffraction. The polymorphic transition of TL was also observed in a fluorescence spectrum. Cascade impactor evaluation on SDPs of TL/HBCD at a 40% ethanol ratio demonstrated high inhalation performance with a fine particle fraction of 33%, while SDPs prepared at a 30% ethanol ratio were lower than that of the others. Regarding the cause of this difference, CFD analysis revealed that high inhalation performance was related to the true density and particle size of SDPs. The change in true density of TL associated with polymorphic transition would affect the inhalation performance. The results on CFD simulations made a prediction about the particle behavior or deposition in pulmonary airways.

Recovering 3D particle size distributions from 2D sections.

We discuss different ways to convert observed, apparent particle size distributions from 2D sections (thin sections, SEM maps on planar surfaces, etc.) into true 3D particle size distributions. We give a simple, flexible and practical method to do this, show which of these techniques gives the most faithful conversions, and provide (online) short computer codes to calculate both 2D-3D recoveries and simulations of 2D observations by random sectioning. The most important systematic bias of 2D sectioning, from the standpoint of most chondrite studies, is an overestimate of the abundance of the larger particles. We show that fairly good recoveries can be achieved from observed size distributions containing 100-300 individual measurements of apparent particle diameter.

Population and hierarchy of active species in gold iron oxide catalysts for carbon monoxide oxidation.

The identity of active species in supported gold catalysts for low temperature carbon monoxide oxidation remains an unsettled debate. With large amounts of experimental evidence supporting theories of either gold nanoparticles or sub-nm gold species being active, it was recently proposed that a size-dependent activity hierarchy should exist. Here we study the diverging catalytic behaviours after heat treatment of Au/FeOx materials prepared via co-precipitation and deposition precipitation methods. After ruling out any support effects, the gold particle size distributions in different catalysts are quantitatively studied using aberration corrected scanning transmission electron microscopy (STEM). A counting protocol is developed to reveal the true particle size distribution from HAADF-STEM images, which reliably includes all the gold species present. Correlation of the populations of the various gold species present with catalysis results demonstrate that a size-dependent activity hierarchy must exist in the Au/FeOx catalyst.

Determination of the surface area and sizes of supported copper nanoparticles through organothiol adsorption—Chemisorption

The mechanisms involving the nanoparticle surfaces in catalytic reactions are more difficult to elucidate due to the nanoparticle surface unevenness, size distributions, and morphological irregularity. True surface area and particle sizes determination are key aspects of the activity of metal nanoparticle catalysts. Here we report on the organothiol adsorption-based technique for the determination of specific surface area of Cu nanoparticles, and their resultant sizes on γ-Al2O3 supports. Quantification of ligand packing density on copper nanoparticles is also reported. The concentration of the probe ligand, 2-mercaptobenzimidazole (2-MBI) before and after immersion of supported copper catalysts was determined by ultraviolet-visible spectrometry (UV–vis). The amount of ligand adsorbed was found to be proportional to the copper nanoparticles surface area. Atomic absorption spectrometry (AAS), N2-physisorption (BET), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA) were used for the characterization of the catalysts. A fair agreement was found between particle sizes obtained from ligand adsorption and TEM methods. The catalytic activity of the copper nanoparticles related to their inherent surface area was evaluated using the model reaction of the oxidation of morin by hydrogen peroxide.

A simplified approach to determine effective surface area and porosity of low bulk density active pharmaceutical ingredients in early development

It can be difficult to accurately measure true density of low bulk density materials, which are frequently used in drug products. This was demonstrated on a crystalline model API. Uncertainty was related to insufficient sample volume. The error function was theoretically described by assuming an inverse relation to the sample volume. Hence, an easy to implement guideline to increase accuracy was established. Verification was performed using spray dried dispersions, SDDs. Practically, bulk density rather than sample volume was used for risk evaluation. Procedures such as compacting a sample into a pellet or using a low volume instrumental calibration mode were implemented. Risk assessment of morphology or crystal form change was included in the guideline.Furthermore, a simplified approach using true density as a central parameter was developed to assess surface area and porosity. For spherically shaped SDDs, surface area can be estimated from true density and particle size, and porosity can be estimated from true and bulk densities. A surface roughness parameter, theoretically derived, leads to a surface area scale factor of 2.28, which provides results in good agreement with the experimentally obtained surface areas. Also, SDD porosities follow a trend similar to those obtained by mercury porosimetry.

In Situ Hard x-Ray Nano-Tomography Study of Lithium Ion Batteries

Lithium-ion batterires (LIBs) are based on insertion reaction chemistry which introduces microstructural changes in host materials via the lithiation and delithation process Particularly, the induced large stain at anode materials (such as widely studied silicon and tin based anodes) can lead to large volume change, fracture, and pulverization, which is considered as a major challenge for anode materials of LIBs (1-2). To address the mechanical degradation requires a fundamental understand of the mechanisms of microstructural change in the electrode as a function of cycling and observing the morphological/structural evolution during the operation of a battery. In-situ measurements have yielded valuable information about the function of electrochemical cells. Since the 3D orientation nature of battery materials in electrodes and possible anisotropy electrochemical reaction, a 3D in-situ visualization technique with nano-scale resolution (battery size requirement) is needed.Synchrotron X-ray imaging is non-destructive, element sensitive, environmental friendly, and highly penetrating. In particular, hard x-ray with high penetration energy holds larger potentials to image micron sized battery materials with a large sample thickness. Our newly-developed TXM at X8C beamline, National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), surpasses the TXMs at other synchrotron facilities in performance, providing nano-scale resolution (sub-30 nm at 2D, sub-50 nm at 3D), local tomography, larger field of view, and automated markerless image acquisition/alignment, which allows for detailed 3D quantitative analysis at nano-scale, including volume change, feature size, curvature, chemical information evolution and stress evaluation (3-5). The major challenge is developing a suitable electrochemical cell which works like a real battery but meet the field of view (40x40 µm), allows a 180-degree rotation without blocking x-ray beam, enables to be sensitive enough to record the current density and measure the electrochemical performance, and undergoes long-term cycling (tens of cycles). Here, we report the implementation of in situ tomography studies of LIBs, aided by a well-designed micron-scaled electrochemical cell consisting of anode particles, a commercial carbonate electrolyte, Li metal as a counter/reference electrode. Different from widely used open nano-battery in in situ TEM study, our designed battery perfectly simulates the true working circumstance and reflect truly the electrochemical reaction in a working LIB. To begin with, our cell allows performing various conventional electrochemical characterizations and analysis. Secondly, replacing carbon paper with conventional Al or Cu foil as the electrode support allows better x-ray penetration, so high-quality tomography with high resolution can be guaranteed. Thirdly, our studying materials are particle shaped (not special nanowire structure) widely applied in battery industries. In addition, our robust battery can undergo considerable stability, and allow long time electrochemical cycling and x-ray characterization.The 3D morphological evolutions of the Sn particles during the first two electrochemical cycles are shown in Fig. 1. In spite of volume expansion, the first lithiated Sn particles mainly keep the overall structure intact. However, severe pulverization and fracture are observed during the first delithiation, when lithium ion extraction and volume shrinkage occur, and during the lithium ion insertion and the volume expansion that occurs in the second lithiation that ensues. After the second lithiation, the particles reach structural equilibrium and no significant changes develop. The fracture and pulverization, on one hand, favor high electrolyte permeation, contributing to lithium ion insertion and associated volume expansion at the second lithiation step. On the other hand, they lead to collapse during the volume expansion that occurs in the second lithiation, thereby few lithium ions are extracted during the second delithiation process. The statistics information at 3D about true volume change, specific area, particle size and curvature will be discussed. A simulation about the stress distribution and the relation to surface curvatures will also be presented. Reference 1. J. Y. Huang et al., Science, 330, 1515 (2010)2. C. K. Chan et al., Nature Nanotech. 3, 31 (2008).3. Y. K. Chen-Wiegart, W. M’ Harris, J. J. Lombardo, W. K. S. Chiu, J. Wang, Appl. Phys. Lett. 2012, 101, 253901.4. J. Wang, Y. K. Chen, Q. Yuan, A. Tkachuk, C. Erdonmez, B. Hornberger, M. Feser, Appl. Phys. Lett. 2012, 100, 143107.5. J. J. Wang,Y. K. Chen-Wiegart, J. Wang, Chem. Commun. DOI:10.1039/C3CC42667J