Lumped-element technique for the measurement of complex density.

A novel lumped-element technique is employed to measure the complex density of a gas in circular pores. The complex density expresses the geometry-dependent viscous coupling between the gas and the pore walls and is related to the thermoacoustic function f(mu), or equivalently, F(lambdaV). The acoustic impedance of a compliant region coupled to a pore (or pore-array) is measured and the impedance of the compliant region is subtracted to yield the impedance of the pore(s) alone, which is directly related to F(lambdaV). Pores of different lengths are measured in order to eliminate end effects. Working down to very low frequencies achieves a wide range of values for the ratio of the viscous penetration depth to the mean pore size. The results agree very well with analytical solutions for circular pores. The technique is also applied to two porous foam materials. Comparing the results to previous measurements of the complex compressibility, it is shown that two different shape factors (or equivalently, characteristic dimensions) are required to account for the data.     

Modeling of heterogeneous surfaces and characterization of porous materials by extending density functional theory for the case of amorphous solids

A method of characterization of carbonaceous materials using nongraphitized carbon black as a reference is considered. The Tarazona density functional theory was applied to amorphous solids to describe nitrogen adsorption on nongraphitized carbon black. This allows us to describe energetic heterogeneity without the need to invoke any energy distribution functions. To derive the pore size distribution (PSD) of porous carbon whose pore walls are non-graphitized, we used the entropy concept in the regularization method. With this approach PSD is more well-behaved than that obtained with the usual means. We applied this new theory to study the effects of technological parameters on porous structure of a series of activated carbon.     

Optimization of STEM-HAADF Electron Tomography Reconstructions by Parameter Selection in Compressed Sensing Total Variation Minimization-Based Algorithms

A novel procedure to optimize the 3D morphological characterization of nanomaterials by means of high angle annular dark field scanning-transmission electron tomography is reported and is successfully applied to the analysis of a metal- and halogen-free ordered mesoporous carbon material. The new method is based on a selection of the two parameters (μ and β) which are key in the reconstruction of tomographic series by means of total variation minimization (TVM). The parameter-selected TVM reconstructions obtained using this approach clearly reveal the porous structure of the carbon-based material as consisting of a network of parallel, straight channels of ≈6 nm diameter ordered in a honeycomb-type arrangement. Such an unusual structure cannot be retrieved from a TVM 3D reconstruction using default reconstruction values. Moreover, segmentation and further quantification of the optimized 3D tomographic reconstruction provide values for different textural parameters, such as pore size distribution and specific pore volume that match very closely with those determined by macroscopic physisorption techniques. The approach developed can be extended to other reconstruction models in which the final result is influenced by parameter choice.     

气孔分布特性对含水多孔介质气体扩散的影响

本文基于多孔介质的气孔分布特性,计算了多孔介质在含水状态下的扩散性能,并且比较了采用两种方式计算相对渗透率时的相对扩散性能。其结果表明,基于气孔分布的计算结果低于与气孔分布无关的计算结果。另外,疏水性含水多孔介质的扩散性能低于亲水性含水多孔介质的扩散性能,基于气孔分布计算含水多孔介质的气体扩散性能时,Wyllie公式并不适用。     

Changes in pore size distribution inside sludge under various ultrasonic conditions

The pore size distribution is quite significant for determining the transport capacity of heat and moisture in sludge during the drying process. It is crucial to investigate the transformation of the pore size in sludge under sonication. In this paper, the microstructures of pores inside sludge before and after ultrasonic treatment with various ultrasonic conditions were observed using a microscope. Fractal geometry and image analysis were combined to quantitatively identify the evolution of pore size in sludge undergoing various acoustic energy densities and treatment times. The surface fractal dimension (d_f) was applied to characterize the pore size distribution of sludge. The results confirmed that sonication has a positive influence on the characteristics of pore structure inside the sludge and that the average pore size increases with increasing ultrasonic energy level, as determined by both acoustic energy density and treatment time. The d_f appropriately characterizes and quantifies the evolution of the pore size distribution of sludge under various ultrasonic conditions. This work is quite valuable for further investigating and evaluating moisture removal in the sludge drying process assisted by ultrasonic treatment.     

An NMR protocol for determining ice crystal size distributions during freezing and pore size distributions during freeze-drying

Nuclear magnetic resonance water proton relaxometry is widely used to investigate pore size distributions and pore connectivity in brine-saturated porous rocks and construction materials. In this paper we show that, by replacing water with acetone, a similar method can be used to probe the porous structure of freeze-dried starch gels and therefore the ice crystal size distribution in frozen starch gels. The method relies on the observation that the starch surface acts as a powerful relaxation sink for acetone proton transverse magnetization so that Brownstein-Tarr theory can be used to extract the pore size distribution from the relaxation data. In addition the relaxation time distribution is found to depend on the spectrometer frequency and the Carr-Purcell-Meiboom-Gill pulse spacing, consistent with the existence of large susceptibility-induced field gradients within the pores. The potential of this approach for noninvasively measuring ice crystal size distributions during freezing and pore size distributions during freeze-drying in other food systems is discussed.     

Fabrication of metal nanodot arrays using a porous alumina membrane as a template

Thin nanodotstructured metal films and heterostructured nanodot arrays (metal nanodot arrays/Si) with a high density and uniform distribution for various kinds of metals (Au, Al, Ag, Pb, Cu, Sn, and Zn) were fabricated by thermal vacuum evaporation using an anodic porous alumina membrane as a template. However, for such metals as Sn, Zn, and Pb with relatively lower melting point as compared with Al it was found that heterostructured nanodot arrays were not formed by a single stage of evaporation. For these metals, we developed a new method termed “two step evaporation method”. The size and the arrays of dots were depended on the pore structure in the anodic porous alumina template. The technique demonstrated in this report is simple and suitable for the preparation of nanodot arrays in the large area for materials which could be vacuum evaporated.     

Characterising the throat diameter of through-pores in network structures using a percolation criterion

We present a method for measuring the pore throat diameter of a simulated porous material. The pore throat diameter is the size of the narrowest pore that has both an entrance and an exit in a network structure. Knowledge of the pore throat diameter allows estimation of the size of the largest molecules that can travel through a network structure without interruption. In this method, a chain of virtual circles (in 2-dimensions) or spheres (in 3-dimensions) is constructed along a percolated path through the pores in a network. The diameter of the largest circle or sphere for which this is possible is the pore throat diameter. The method is applied to two 2-dimensional models (one where we know the pore throat diameter and one where we do not), and well predicts the pore throat diameters in each case. The pore throat diameter of a 3-dimensional DNA-mediated hydrogel model is also determined. This method is applicable to any porous structure for which molecular coordinate information is available. The ability to predict pore throat diameters in simulation could be useful for determining the size of molecules that can safely be administered by hydrogel drug delivery systems.     

Xenon porometry: a novel method for the derivation of pore size distributions

Xenon porometry is a novel method used for characterizing porous materials by the (129)Xe nuclear magnetic resonance of xenon gas. With the method, the diffusion of gas is slowed down by immersing the material in a medium, which can be in liquid or solid state during measurements. Because of slow diffusion, the signal of a xenon atom is characteristic of the properties of only one pore, and the composite signal of all atoms represents the distribution of properties. The method is especially applicable for determining pore size distribution because the chemical shifts of two different xenon signals (one from liquid and the other from gas pockets in solid) are dependent on pore size. Therefore, the shapes of these signals represent pore size distribution function. In addition, the porosity of the material can be determined by comparing the intensities of two signals. This article focuses on describing xenon signals observed from gas pockets in a solid medium, which has turned out to be most convenient for pore size determination.     

Magnetic resonance imaging by synergistic diffusion-diffraction patterns

Inferring on the geometry of an object from its frequency spectrum is highly appealing since the object could then be imaged noninvasively or from a distance (as famously put by Kac, "can one hear the shape of a drum?"). In nuclear magnetic resonance of porous systems, the shape of the drum is represented by the pore density function that bears all the information on the collective pore microstructure. So far, conventional magnetic resonance imaging (MRI) could only detect the pore autocorrelation function, which inherently obscures fine details on the pore structure. Here, for the first time, we report on a unique imaging mechanism arising from synergistic diffusion-diffractions that directly yields the pore density function. This mechanism offers substantially higher spatial resolution compared to conventional MRI while retaining all fine details on the collective pore morphology. Thus, using these unique synergistic diffusion-diffractions, the "shape of the drum" can be inferred.     

Dielectric constant of porous ultra low-k dielectrics by fractal-Monte Carlo simulations

The effective dielectric constant of porous ultra low-k dielectrics is simulated by applying the fractal geometry and Monte Carlo technique in this work. Based on the fractal character of pore size distribution in porous media, the probability models for pore diameter and for effective dielectric constant are derived. The proposed model for the effective dielectric constant is expressed as a function of the dielectric coefficient of base medium and the volume fractions of pores and base medium, fractal dimension for pores, the pore size, as well as random number. The Monte Carlo simulations combined with the fractal geometry are performed. The predictions by the present simulations are shown in good accord with the available experimental data. The proposed technique may have the potential in analyzing other properties such as electrical conductivity and thermal conductivity in porous ultra low-k dielectrics.     

Gradient porous alumina films with different pore distributions by anodization of aluminum

In this paper, gradient porous alumina films with different pore distributions are fabricated by asymmetrical anodization of Al foils. When an insulating baffle is inserted close to the anode, depending on the shape of the baffle, the current density distribution on the Al foils can be varied. Two kinds of porous alumina films with different pore distributions are fabricated by this method. This bottom-up approach of asymmetrical anodization of Al foil provides us with a low-cost method to fabricate large-size gradient porous structures with different pore distributions.     

Comparison of NMR simulations of porous media derived from analytical and voxelized representations

We develop and compare two formulations of the random-walk method, grain-based and voxel-based, to simulate the nuclear-magnetic-resonance (NMR) response of fluids contained in various models of porous media. The grain-based approach uses a spherical grain pack as input, where the solid surface is analytically defined without an approximation. In the voxel-based approach, the input is a computer-tomography or computer-generated image of reconstructed porous media. Implementation of the two approaches is largely the same, except for the representation of porous media. For comparison, both approaches are applied to various analytical and digitized models of porous media: isolated spherical pore, simple cubic packing of spheres, and random packings of monodisperse and polydisperse spheres. We find that spin magnetization decays much faster in the digitized models than in their analytical counterparts. The difference in decay rate relates to the overestimation of surface area due to the discretization of the sample; it cannot be eliminated even if the voxel size decreases. However, once considering the effect of surface-area increase in the simulation of surface relaxation, good quantitative agreement is found between the two approaches. Different grain or pore shapes entail different rates of increase of surface area, whereupon we emphasize that the value of the “surface-area-corrected” coefficient may not be universal. Using an example of X-ray-CT image of Fontainebleau rock sample, we show that voxel size has a significant effect on the calculated surface area and, therefore, on the numerically simulated magnetization response.     

基于Biot-喷射流统一模型Maxwell流体饱和孔隙介质中的弹性波

推广Biot-Tsiklauri声学模型的同时借鉴Dvorkin和Nur的工作,建立了具有任意孔径分布并顾及喷射流动机制的非牛顿流体饱和孔隙介质声学模型,研究了非牛顿流体(Maxwell流体)饱和孔隙介质中的弹性波的衰减和频散特性.着重讨论充孔隙Maxwell流体的非牛顿流效应对弹性波的频散和衰减的影响.研究表明,饱和流体的非牛顿流效应和喷射流动机制均是引起弹性波波频散和衰减的重要因素.依据非牛顿流体(Maxwell流体)饱和各向同性孔隙介质的Biot-喷射流声学模型,喷射流动只影响纵波的频散和衰减,而饱和流体的非牛顿流效应不仅影响纵波,而且还影响横波的频散和衰减.     

Pore size distribution in porous glass: fractal dimension obtained by calorimetry

By differential Scanning Calorimetry (DSC), at low heating rate and using a technique of fractionation, we have measured the equilibrium DSC signal (heat flow) J _q ⁰ of two families of porous glass saturated with water. The shape of the DSC peak obtained by these techniques is dependent on the sizes distribution of the pores. For porous glass with large pore size distribution, obtained by sol-gel technology, we show that in the domain of ice melting, the heat flow J_q is related to the melting temperature depression of the solvent, ΔT _m , by the scaling law: J _q ⁰∼ΔT _m ^{- (1 + D)}. We suggest that the exponent D is of the order of the fractal dimension of the backbone of the pore network and we discuss the influence of the variation of the melting enthalpy with the temperature on the value of this exponent. Similar D values were obtained from small angle neutron scattering and electronic energy transfer measurements on similar porous glass. The proposed scaling law is explained if one assumes that the pore size distribution is self similar. In porous glass obtained from mesomorphic copolymers, the pore size distribution is very sharp and therefore this law is not observed. One concludes that DSC, at low heating rate ( q? 2^°C/min) is the most rapid and less expensive method for determining the pore distribution and the fractal exponent of a porous material. Received 23 July 1999 and Received in final form 16 February 2001     

Noise control of a rectangular cavity using macro perforated poro-elastic materials

The effectiveness of macro perforated porous materials to control noise levels inside a cavity is investigated. This is done using a finite element formulation based on the Biot-Allard theory that accounts for sound propagation in a poro-elastic medium. Earlier investigations have shown that macro-holes in a porous material can enhance low frequency sound absorption. However, this has been demonstrated in free field or waveguide environments. When such an approach is used in a cavity, it is seen that only certain patterns of macro-holes, dictated by cavity mode shapes, enhance noise reduction in the higher frequency ranges. This phenomenon is shown to be independent of porous material properties by considering two different materials. A correlation between the mode shapes and material removal is also established. A detailed convergence study for both cavity and poro-elastic finite element models, establishes the suitability of using higher order interpolation functions for coupled cavity-poro-elastic acoustic analysis.     

Fabrication of the uniform CdTe quantum dot array on GaAs substrate utilizing nanoporous alumina masks

Fabrication of quantum dot array (QDA) is attractive for applications in electronic and optoelectronic devices. The CdTe QDAs have potential applications in optoelectronic devices of visible range. One of the major challenges in fabricating QDAs is the uniformity and reproducibility in size and spatial distribution. The uniformity and reproducibility of QDs can be improved by using the nanoporous alumina mask. The geometry of porous alumina is schematically represented as a close-packed array of columnar hexagonal cells, each containing a central pore normal to the substrate. The well-ordered nanoporous alumina masks were able to obtain by two-step anodizing processes from aluminum in oxalic acid solutions at low temperature. The pore size, thickness, and density of nanoporous alumina mask can be controlled with the anodization voltage, time, and electrolyte. The CdTe QDAs on the GaAs substrate was grown by molecular beam epitaxy method using the porous alumina masks. The temperature of substrate and source (Cd, Te) was an important factor for the growth of CdTe QDs on GaAs substrate. The CdTe QDAs of 80 nm dot size was fabricated; using the porous alumina masks (300 nm thickness) of pore diameter (80 nm) and density (10¹⁰ /cm²).     

Characterization of multi-scale porous structure of fly ash/phosphate geopolymer hollow sphere structures: From submillimeter to nano-scale

In the present work, the porous structure of fly ash/phosphate geopolymer hollow sphere structures (FPGHSS), prepared by pre-bonding and curing technology, has been characterized by multi-resolution methods from sub-millimeter to nano-scale. Micro-CT and confocal microscopy could provide the macroscopic distribution of porous structure on sub-millimeter scale, and hollow fly ashes with sphere shape and several sub-millimeter open cells with irregular shape were identified. SEM is more suitable to illustrate the distribution of micro-sized open and closed cells, and it was found that the open cells of FPGHSS were mainly formed in the interstitial porosity between fly ashes. Mercury porosimeter measurement showed that the micro-sized open cell of FPGHSS demonstrated a normal/bimodal distribution, and the peaks of pore size distribution were mainly around 100 and 10 μm. TEM observation revealed that the phosphate geopolymer was mainly composed of the porous area with nano-pores and dense areas, which were amorphous Al–O–P phase and α-Al₂O₃ respectively. The pore size of nano-pores demonstrated a quasi-normal distribution from about 10 to 100 nm. Therefore, detailed information of the porous structure of FPGHSS could be revealed using multiple methods.