Production of finely ground natural graphite particles with high electrical conductivity by controlling the grinding atmosphere

Natural graphite particles with high crystallinity sieved to obtain a particle size range of under 63 μm were ground with a ball mill, under various well-controlled grinding atmospheres such as N₂, O₂, He, H₂, and vacuum. The ratio, X_dif50/X_st50, i.e. between the 50 wt.% Stokes diameter and the 50 wt.% laser diffraction diameter, of the ground particles, was used as an index of the flakiness of the particles. The specific resistance of films composed of the ground graphite particles was systematically measured. The rate of reduction in the size of the particles by grinding was slow under an O₂-rich atmosphere such as 100% O₂ and dry air. On the other hand, it was relatively fast in vacuum, or under an N₂ or He atmosphere, and a gas mixture of 99% N₂ and 1% O₂. The rate of size reduction by grinding under a H₂ atmosphere was intermediate. In our experimental conditions, the flakiness of the ground particles increased with the decrease in the particles’ sizes. The electrical conductivity of the ground particles, however, tended to decrease with the decrease in their sizes. Under the condition that the Stokes diameter of the ground particles remains constant, the electrical conductivity of films made from the ground particles increases with the increase in the flakiness of the particles. It was finally determined from our systematic grinding experiments that small flaky particles, which had a size, X_st of ∼1 μm, with a high electrical conductivity can be produced by grinding in a gas mixture of 99% N₂ and 1% O₂. In this case, the flaky shape of the ground particles was visually confirmed by scanning electron microscopy.     

Partikelform und Porosität von biogenen Pyrolysekoksen

Char particles from pyrolyzed biomass vary in particle size and shape. On average, the particles are more elongated the larger their size. The average size‐specific elongation is almost alike for all investigated samples, i.e. independent from their source material and process. The particle collectives cannot be characterized accurately with classical particle size distributions, which assume spherical particle shape. Accounting for their shape, they can be described more accurately with particle size distributions that are based on an ellipsoid model. The high bulk porosity is mainly attributed to the spaces between particles.     

Evaluation of DMA Size Selection of Dry Dispersed Mineral Dust Particles

Mineral dust particles play a significant role in the Earth's radiative balance via direct interaction with solar radiation and indirectly through their ability to initiate cloud formation. Many field and laboratory studies utilize a differential mobility analyzer (DMA) for particle size selection. Here we evaluate the use of a DMA to size-segregate dry dispersed mineral dust particles. We examine the post-DMA size distribution using four different techniques: a scanning mobility particle sizer (SMPS) for mobility sizing, an optical particle sizer (OPS) for optical sizing, the Particle Analysis by Laser Mass Spectrometry (PALMS) instrument for vacuum aerodynamic sizing, and electron microscopy (EM) for geometric sizing. While the SMPS measured a narrow mobility size distribution at the DMA-selected diameter, the OPS, PALMS, and EM in most cases showed broader distributions and a smaller mode size than that selected by the DMA. These techniques also observed super-micrometer particles, often extending beyond the upper size limit of a typical SMPS scan. Complicating analysis, particle shape factor (χ) was observed to be a function of mobility size, ranging from 1.3 at 500 nm to 3.1 at 1000 nm. We conclude that mobility size selection of mineral dust particles using a DMA most often does not yield particles of the desired physical size or surface area. We suggest that attempts to size-select from a broad distribution of non-spherical particles require an independent measurement downstream of the DMA to verify the actual selected size.

Copyright 2015 American Association for Aerosol Research     

CALIBRATION OF A WHITE-LIGHT/90° OPTICAL PARTICLE COUNTER FOR “AERODYNAMIC” SIZE MEASUREMENTS—EXPERIMENTS AND CALCULATIONS FOR SPHERICAL PARTICLES AND QUARTZ DUST

This paper describes the calibration of an optical particle counter with the help of an aerodynamic particle sizer. The calibration method and influencing errors are discussed. The transfer characteristic of the optical particle counter is determined with monodisperse fractions of polystyrene latex spheres and verified with spherical particles (glycerine) of known refractive index. In calibration experiments with three optical particle counters of the same type the method proved to be transferable to different devices. The described method was validated for nonspherical particles (quartz). The results from calibration by means of an aerodynamic particle sizer are in perfect agreement with the results from calibration by means of sampling cyclones. The enhancement of scattered light intensity due to irregular particle shape is demonstrated by the comparison of experimental quartz calibrations with calculations for spherical quartz particles.     

Exhaust Particle Size Distribution Measurements at the Tuscarora Mountain Tunnel

On-road particle size distributions were measured at the Tuscarora Mountain tunnel on the Pennsylvania Turnpike in May 1999. The data were obtained using a scanning mobility particle sizer. The nucleation modes of the size distributions contained most of the particles on a number concentration basis and exhibited peak diameters ranging from 11 to 17 nm. This observation is consistent with previous calculations and measurements, indicating that significant numbers of ultrafine aerosol particles can be expected in close proximity to busy motorways. The experiment provided 4 case studies for which the tunnel inlet data could be used to correct data obtained at the outlet, allowing for estimates of particle production within the tunnel. Exhaust particle production rates per vehicle kilometer were estimated; the results are presented with the caveat that the measurements were affected by ambient dilution. The 4 case study nucleation mode sizes varied inversely with ambient temperature. The light-duty vehicle contributions to the ultrafine particle distributions were apparently dominated by the heavy-duty vehicle contributions.     

Analysis and evaluation of permeability techniques for characterizing fine particles Part II. Measurement of specific surface area

The performance of both steady-state and transient permeameters has been evaluated. A number of standard powders was chosen and their surface areas determined by gas adsorption techniques for comparison with surface areas obtained using permeameters. The powders were chosen to cover a wide range o density (0.92 – 18.7 g/cm³) and surface area (0.06 – 350 m²/g).The effect of particle shape, i.e. needles, spherical particles, flakes and irregularly shaped particles on surface area determined by permeametry has also been studied. A linear relationship between BET surface area and that obtained by using a simple U-tube transient flow permeameter has been obtained over a wide range of particle size and macroporosity.The Fisher Subsieve Sizer was chosen as a typical example of a steady-state permeameter, and a number of shortcomings in this instrument have been found. A simple steady-state permeameter was constructed to evaluate the theoretical model as developed in Part I for atmospheric pressure permeametry, and the model has been found to give good values of external surface areas for powders having an average particle size greater than 2 μm. The effect of slip flow for particles less than 1 μm in diameter has been established for atmospheric pressure permeametry.This paper also presents measurements of specific surface area determined by using a more recent permeameter, namely the Permaran. This instrument performed within a reproducibility of ±7% and produced data in agreement with that taken on similar devices and also with the theoretical analysis presented in Part I.The performance of a Knudsen-flow permeameter has been evaluated, and the instrument has been found to give accurate values of external surface area of fine as well as coarse powders.     

Evolution of asphaltene floc size distribution in organic solvents under shear

A mathematical model was developed on the basis of population balance to analyze experimental data on asphaltene floc size distribution in a coagulating suspension. Experiments were carried out in a Couette device under a laminar flow condition. Floc size distributions were measured on-line using optical microscopy and image analysis. The aggregation behavior of asphaltenes was investigated by monitoring the size distribution of flocs for various intensities of agitation (i.e., shear rate, G), solvent composition (i.e., ratio of toluene to n-heptane in the solution, T:H) and particle contents (i.e., volume fraction of particles, ?). The results showed that (i) the floc size distribution can be predicted using a population balance approach, (ii) a steady-state mean floc size is reached for a given shear rate, and (iii) this steady-state floc size increases as ? is increased or T:H is reduced. The relative rates of shear-induced aggregation and fragmentation determine the steady-state size distribution. Similar floc size distributions were obtained at steady state for various shear rates, indicating that the width of the size distribution is independent of shear. However, the experimental observations indicate that the steady-state floc size distribution depends on asphaltene concentration and solvent composition.     

Synthesis and characterization of monodisperse uniformly shaped respirable aerosols

The top‐down, micromolding technique, referred to as Particle Replication in Nonwetting Templates (PRINT^®), affords a new opportunity for the generation of inhalation therapeutics. Powders were fabricated with predetermined particle size and shape; when dispersed with a collision jet nebulizer, these particles resulted in monodisperse aerosols with geometric standard deviations well below 1.2. Dynamic shape factors for this novel set of uniformly shaped particles were determined by correcting the drag of nonspherical particles in the ultra‐Stokesian flow conditions of the aerodynamic particle sizer (APS). This convenient approach for shape factor determination agreed well with current literature approaches and allowed for the correction of APS results for particles with known volumes. Determined shape factor values of PRINT geometries were used to estimate the theoretical median aerodynamic diameters of individual aerosols, which were then compared to actual inhalation powders. © 2013 American Institute of Chemical Engineers AIChE J, 59: 3184–3194, 2013     

A Newly Designed and Constructed Instrument for Coupled Infrared Extinction and Size Distribution Measurements of Aerosols

Although atmospheric particles are often non-spherical, Mie theory is commonly used to acquire aerosol optical depth, composition, and transport information from satellite retrievals. In the infrared (IR) region, the radiative effects of aerosols, usually modeled with Mie theory, are subtracted from satellite spectral data to determine key atmospheric and oceanic properties. To gain a better understanding of the infrared radiative effects of aerosols and the methods used to model them, an instrument has been designed to simultaneously measure infrared extinction spectra and particle size distributions obtained from a scanning mobility particle sizer (SMPS) and an aerodynamic particle sizer (APS). Infrared extinction spectra are simulated with Mie theory using the measured particle size distributions and available literature optical constants. As a result, the errors associated with using Mie theory to model the infrared extinction of mineral dust aerosol can be quantitatively examined. Initial results for this instrument are presented here. For ammonium sulfate, the Mie theory simulation is in good agreement with our measured extinction spectrum. This is in accordance with the nearly spherical shape of ammonium sulfate particles. However, for illite, an abundant clay mineral, there is poor agreement between the experimental spectrum and the Mie simulation. This result is attributed to particle shape effects.     

A new miniature electrical aerosol spectrometer (MEAS): Experimental characterization

Design and theory of a new compact ultrafine particle sizing instrument, called the miniature electrical-mobility aerosol spectrometer (MEAS), was recently introduced [Ranjan, M., & Dhaniyala, S. (2007). A new miniature electrical spectrometer: Theory and design. Journal of Aerosol Science, 39, 950–963]. In the MEAS, electrostatic precipitation technique is used for both generation of sheath flow and classification of particles based on their electrical mobility. An electrometer-array, connected to the collection electrodes in the classifier section, is used to measure the number of particles collected in the different mobility channels, and these data are inverted using MEAS transfer functions to obtain particle number size distributions. Design of a prototype MEAS and the experimental approach to validate the performance of the individual components of the instrument are presented. Particle size distributions obtained from MEAS measurements compare well with those obtained using a scanning mobility particle sizer (SMPS; TSI 3936), validating theoretical calculations of instrument transfer functions. The operational limits of MEAS are determined from the calculation of error in the inverted size distribution as a function of total particle concentration. This analysis suggests that the designed MEAS can be used for applications such as personal and ambient monitoring under conditions of moderate to high particle concentrations.     

The formation of incense smoke

The formation of incense smoke generated from four different types of incense sticks, three manufactured in Taiwan and one in Japan, was investigated in a small controlled chamber. The scanning mobility particle sizer and the quartz crystal microbalance were used for particle size analyses. The count median diameter (CMD) was found to rise swiftly along the path of the incense smoke. Consequently, a representative sampling location was selected for all measurements performed thereafter. All four types of incense smoke were shown to exhibit characteristic size distributions, CMDs, and mass median aerodynamic diameters (MMADs). Electron microscopy depicted liquid and solid nature of Taiwan and Japan incense smoke, respectively. The different physical states of the particles were suspected to be a result of different smoke-generating ingredients used by different cultures. Finally, the formation mechanisms of both liquid and solid incense smoke were discussed.     

Particle Size Distribution of Coprecipitated Mn-Zn Ferrite Powders

The particle size distribution of 0.07- to 0.35-μm powders was measured by quantitative electron microscopy using an areal analysis. Measurements of at least 15 particles were required to characterize each size distribution. The specific surface area calculated from the size distributions satisfactorily agreed with that measured by the BET method. For the powders with surface area of 4.4 to 9.7 m²/g, the particle size distributions were generally narrow. In many cases the distributions were near log normal.     

Melting salt assisted sol–gel synthesis of blue phosphor Y2SiO5:Ce

High brightness Y₂SiO₅:Ce phosphor powders with spherical shape and fine size were synthesized by melting salt assisted sol–gel method (MS&Sol–Gel). Commercial tetraethyl orthosilicate was used as the silica source and rare earth oxides were used as rare earth source. The prepared Y₂SiO₅:Ce powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), laser particle sizer, and fluorescentometer techniques. Y₂SiO₅:Ce powders were obtained at significantly lower temperature than that by conventional techniques. When sintered at 1200 °C for 2 h with 5 wt.% LiF and 2 wt.% KH₂PO₄ as fluxes, particles with spherical shape and narrow particle distribution could be obtained. Moreover, the grain size of the powders prepared through this process was in the range of 2–7 μm, strongly depending on the thermal treatments and the species of fluxes. PL intensity of the prepared Y₂SiO₅:Ce phosphor using 5 wt.% LiF and 2 wt.% KH₂PO₄ as fluxes was similar to that of commercial product.     

Gas-to-Particle Conversion in the Particle Precipitation–Aided Chemical Vapor Deposition Process II. Synthesis of the Perovskite Oxide Yttrium Chromite

In the particle precipitation-aided chemical vapor deposition process, an aerosol is formed in the gas phase at elevated temperatures. The particles are deposited on a cooled substrate. Coherent layers with a controlled porosity can be obtained by a simultaneous heterogeneous reaction, which interconnects the deposited particles. The synthesis of submicrometer powder of the perovskite oxide yttrium chromite (YCrO₃) by gas to particle conversion, which is the first step of the PP-CVD process, has been investigated, and preliminary results are shown. The powders have been synthesized using yttrium trichloride vapor (YCl₃), chromium trichloride vapor (CrCl₃), and steam and oxygen as reactants. The influence of the input molar ratio of the elements on the composition and characteristics of the powders has been investigated. Phase composition has been determined by X-ray diffraction (XRD). The powders have been characterized by transmission electron microscopy (TEM) and sedimentation field flow fractionation (SF³). At a reaction temperature of 1283 K the powders consist of chromium sesquioxide (Cr₂O₃), or a mixture of Cr₂O₃ and YCrO₃. At stoichiometric input amounts of metal chlorides and steam the formation of YCrO₃ seems to be favored. Two typical particle size distributions have been observed. The primary particle size ranges from 5 to 30 nm for small particles, and from 40 to 250 nm for large particles, depending on the process conditions. The particles tend to be agglomerated. The weight of the agglomerates is independent of the primary particle diameter.     

Hydrothermal Synthesis of Nanosized Titania Powders: Influence of Tetraalkyl Ammonium Hydroxides on Particle Characteristics

Three types of tetraalkyl ammonium hydroxides (TANOHs)—namely, tetramethyl ammonium hydroxide (TMNOH), tetraethyl ammonium hydroxide (TENOH), and tetrabutyl ammonium hydroxide (TBNOH)—were used as peptizing agents for the hydrothermal synthesis of nanocrystalline TiO₂ powders. X-ray diffractometry, Brunauer-Emmett-Teller surface-area analysis, differential thermal analysis-thermogravimetry, scanning electron microscopy, and transmission electron microscopy were used to characterize the powders. The results showed that the carbon-chain length of TANOHs had a great influence on the particle size, particle shape, and the phase transformation of the hydrothermally derived TiO₂ particles. Anatase phase was obtained in all the samples, regardless of the peptizer used, and the particle size increased as the peptizer cation size decreased. In the presence of TMNOH, the particle shape changed from spherical at low concentration to rodlike with increasing TMNOH concentration, whereas a transition from a spherical morphology to an asterisk-like structure was observed in the TENOH peptized samples. However, spherical particles were formed in all the TBNOH peptized samples. The anatase-rutile transition occurred at a lower temperature for the TENOH-derived powders, relative to the other two peptizers.     

Measuring aerosol size distributions with the fast integrated mobility spectrometer

A fast integrated mobility spectrometer (FIMS) has been developed for rapid aerosol size distribution measurements including those aerosols with low particle number concentrations. In this work, an inversion routine has been developed for the FIMS and it is demonstrated that the FIMS can accurately measure aerosol size distributions. The inversion routine includes corrections for the particle residence time in the FIMS and other factors related to the width of the response (or transfer) function and multiple charging of particles. Steady-state size distributions measured with the FIMS compared well with those measured by a scanning mobility particle sizer (SMPS). Experiments also show that the FIMS is able to capture the size distribution of rapidly changing aerosol populations. The total particle concentration integrated from distributions measured by the FIMS agrees well with simultaneous measurements by a condensation particle counter (CPC).     

Experimental investigation of pressure drop in packed beds of irregular shaped wood particles

The knowledge of the pressure drop across a packed bed of irregular shaped wood particles is of great importance for achieving optimal control and maximum efficiency in many applications, such as wood drying, pyrolysis, gasification and combustion. In this work the effect of porosity, average particle size and main particle orientation on the pressure drop in a packed bed is investigated. To this end, particle size distributions and porosities are determined experimentally.Based on the experimental results obtained in this study, the form coefficient C and the permeability K of the Forcheimer equation are calculated for different packed beds. The Ergun equation requires an average equivalent particle diameter that is derived from the measured particle size distribution. This equivalent diameter and the corresponding bed porosity are used in the well known Ergun equation in order to derive adapted shape factors A and B.Since a change in bed porosity and particle size, caused by the degradation of the wood particles and gravity, can be expected in a reacting packed bed, a set of shape factors for use with the Ergun equation is determined that are independent of porosity and particle diameter and fit the experimental data very well.     

Size segregation in gas-solid fluidized beds with continuous size distributions

Discrete-particle simulations of a gas-solid fluidized bed are used to investigate the species segregation (de-mixing) behavior of systems with continuous particle size distributions. Both Gaussian and lognormal distributions are investigated over a range of distribution widths, restitution and friction coefficients, and gas velocities. The results indicate that: (i) the average particle diameter decreases as the height within the bed increases, (ii) the level of segregation increases with an increase in the width of the particle size distribution, and (iii) segregation is attenuated as bubbling becomes more vigorous. Furthermore, the shape of the local size distribution (i.e., Gaussian or lognormal) is found to mimic that of the overall size distribution in most regions of the fluidized bed.     

Aerosol Generation of Nonspherical Particles by Desublimation of Copper Phthalocyanine

A novel generator for a defined test aerosol consisting of nonspherical particles was developed based on the desublimation of copper phthalocyanine during adiabatic cooling. Employing a brush disperser, copper phthalocyanine powder is dosed and dispersed in a nitrogen flow and sublimated in a tube furnace. Downstream the furnace new particles are formed due to the adiabatic expansion and the desublimation of the material in a laval nozzle. The generated particles were characterized employing a scanning mobility particle sizer and an aerosol particle mass analyzer to determine the size distribution and the dynamic shape factor. For the operating parameters of the generator examined here, particles with a mobility diameter between 30 and 600 nm were generated. The measured values for the dynamic shape factor of the particles were confirmed by scanning electron microscopy analysis.