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.     

Ultrasound induced formation of paraffin emulsion droplets as template for the preparation of porous zirconia

The paraffin particles were prepared by quenching process after sonicating the solution of paraffin and water at 80 °C. The resultant paraffin particles were then used as template for the preparation of macroporous zirconia materials. For this, zirconium normal butoxide (ZNB) modified with triethanolamine (TEA) was first hydrolyzed by water containing the dispersed paraffin particles with the surfactant, Sodium di(2-ethylhexyl) sulfosuccinate. This resulted in the formation of a slurry consisting of hydrolyzed sol and paraffin particles. After centrifugation, a cake packed with hydrated sol and paraffin particles were obtained which was then subjected to heat treatment. The sample obtained after heat treatment contained finely dispersed pores in the size range from 40 nm to 2 μm. Moreover, using the present approach it has also been observed that, change in pore size of zirconia wall is possible with a change in size of the paraffin particles. Thus, the present approach is a novel way of producing porous materials as the particle size of the template could be changed and templates become hard when they were molded as compared to the conventional methods in which there is no change in phase for the templates under 100 °C.     

Air Flow in Aluminum Foam: Heat Transfer and Pressure Drops Measurements

Abstract

Metal foams are cellular structure materials that present open cells, randomly oriented and mostly homogeneous in size and shape. Cellular structure materials, and particularly open-cell metal foams, have been proposed as possible substitutes for traditional finned surfaces in electronics cooling applications. This article presents the heat transfer and pressure drops measurements obtained during air flow through an aluminum foam, which has 40 pores per inch with 0.63 mm pore diameter. The specimen has been inserted in a new open-circuit type wind channel with a rectangular cross-section that has recently been built at the Department of Fisica Tecnica of the University of Padova. The experimental heat transfer coefficients and pressure drops have been collected by varying the air flow rate supplied by the screw compressor that provides a variable volumetric air flow ranging between 0–90 m³h^?1 at a constant gauge pressure of 7 bar. The specific heat flux has been simulated by powering with a 25-kWm^?2 copper heater attached at the bottom of the aluminum foam base plate. The experimental results are reported in terms of heat transfer coefficients, mean normalized wall temperatures, and pressure drops.     

Specific heat of nanostructured superconducting tin in magnetic fields

Specific heat of tin nanoparticles, which are embedded in porous glass with average pore size ～7 nm, has been investigated in the low-temperature region in magnetic fields up to 2 T. The temperatures of the transition into the superconducting state in various magnetic fields have been determined for tin nanostructured in porous glass. The H _c -T _c phase diagram has been constructed. The upper critical field has been evaluated and the electronic specific heat coefficient and the Debye temperature have been refined. These results have been discussed within the structural model of tin nanoparticles in porous glass.     

Segmental dynamics of poly(methyl phenyl siloxane) confined to nanoporous glasses

The effect of a nanometer confinement on the molecular dynamics of poly(methyl phenyl siloxane) (PMPS) was studied by dielectric spectroscopy (DS), temperature modulated DSC (TMDSC) and neutron scattering (NS). Nanoporous glasses with pore sizes of 2.5–20 nm have been used. DS and TMDSC experiments show that for PMPS in 7.5 nm pores the molecular dynamics is faster than in the bulk which originates from an inherent length scale of the underlying molecular motions. For high temperatures the temperature dependence of the relaxation rates for confined PMPS crosses that of the bulk state. Besides finite states effects also the thermodynamic state of nano-confined PMPS is different from that of the bulk. At a pore size of 5 nm the temperature dependence of the relaxation times changes from a Vogel/Fulcher/Tammann like to an Arrhenius behavior where the activation energy depends on pore size. This is in agreement with the results obtained by NS. The increment of the specific heat capacity at the glass transition depends strongly on pore size and vanishes at a finite length scale between 3 and 5 nm which can be regarded as minimal length scale for glass transition to appear in PMPS.     

泡沫铝翅片传热和流动特性的实验研究

对泡沫铝翅片传热和流动特性进行了实验研究,泡沫铝的空隙率为0.90,孔密度(PPI)分别为10,20,40。实验结果表明,孔密度较大时,传热系数也较大,但流动阻力系数也明显升高。通过引入无因次变量Dα,得到了泡沫铝翅片的流动阻力系数和传热的初步准则关联式。     

Effect of porosity and pore morphology on the low-frequency dielectric response in sintered ZrO<Subscript>2</Subscript>—8 mol% Y<Subscript>2</Subscript>O<Subscript>3</Subscript> ceramic compact

Effect of porosity and pore size distribution on the low-frequency dielectric response, in the range 0.01–100 kHz, in sintered ZrO₂—8 mol% Y₂O₃ ceramic compacts have been investigated. Small-angle neutron scattering (SANS) technique has been employed to obtain the pore characteristics like pore size distribution, specific surface area etc. It has been observed that the real and the imaginary parts of the complex dielectric permittivity, for the specimens, depend not only on the porosity but also on the pore size distribution and pore morphology significantly. Unlike normal Debye relaxation process, where the loss tangent vis-à-vis the imaginary part of the dielectric constant shows a pronounced peak, in the present case the same increases at lower frequency region and an anomalous non-Debye type relaxation process manifests.     

去合金化工艺对纳米多孔铜纯度的影响

采用腐蚀去合金化方法制备纳米多孔铜材料。研究了固溶时间、腐蚀时间及腐蚀温度对纳米多孔铜表面形貌及残余Mn含量的影响。研究表明:由于固溶时间的延长，合金成分越来越均匀化，去合金化后所得纳米多孔铜的残余Mn原子分数降低。固溶95 h的前驱体合金，随着腐蚀时间的延长，其残余Mn含量降低不明显；随着温度的升高，其残余Mn原子分数由25 ℃的3.54%降至60℃的1.14%，但是60 ℃腐蚀后的孔隙与丝径尺寸明显粗化，样品易碎。通过调整去合金化参数，实验所制备的纳米多孔铜呈现均匀的海绵状纳米多孔结构，残余Mn原子分数1.23%, 平均丝径尺寸40 nm。     

On preparation of fine particles of MnFe2O4 and their magnetic properties

Influence of the heat treatment, following a wet chemical process, has been examined on the sizes of the obtained particles of MnFe₂O₄. X-ray diffraction, magnetization and Mössbauer measurements have been used. The average sizes of the obtained particles are in the range of ～ 100 Å–300Å with the upper size limit being ～ 450 Å and more. The average size as well as size distribution is strongly influenced by the nature of the heat treatment followed for preparation of the sample. Prolonged hydrothermal heating resulted in larger average size than did dry heating at 400°C of the precipitate obtained from the initial wet process. Further dry heating following hydrothermal treatment did not lead to any major growth. Chemical nature of the starting materials also affects the sizes.     

Heat of adsorption and density distribution in slit pores with defective walls: GCMC simulation studies and comparison with experimental data

The adsorption behavior (capacity, density distribution and packing density) and the isosteric heat versus loading in a slit pore whose walls contain defective graphene layers are investigated in this paper. The defective wall is characterized by the extent and size of the defect. Simulation results obtained with the Grand Canonical Monte Carlo method reveal complex patterns of isosteric heat, and this complex behavior is a result of the interplay between three factors: (i) the surface heterogeneity (solid-fluid interaction, sites with varying degree of affinity), (ii) fluid-fluid interaction and (iii) the overlapping of potentials exerted by the two defective walls. We illustrate this with argon adsorption in pores of various sizes, and results obtained from the simulation agree qualitatively with the experimental data at 77 K on Saran microporous S600H and micro-mesoporous S84 charcoals of Beebe et al. [R.A. Beebe, B. Millard, J. Cynarski, J. Am. Chem. Soc. 75 (1953) 839]. The S600H was found to contain pores predominantly in the neighborhood of 7 Å with 30% of defect and a defective size of 2.84 Å. This is consistent with the argument made by Beebe et al. that this sample is a microporous solid and most pores can accommodate only one layer. The other sample, S84, has larger pores than S600H, and it is found that it has a wider pore size distribution and the pore width is centered at about 12 Å.     

Vacuum Calcination Behavior of SBA-15 Ordered Mesoporous Silica

In this paper, the calcination of SBA-15 in vacuum is followed by in situ and ex situ small angle X-ray scattering (SAXS) measurements at different temperatures and the material properties are compared with the conventional calcination process in nitrogen and air. The whole process of template decomposition and by-products elimination is investigated as a function of temperature, showing early stages of polymer decomposition at 200 °C. The textural properties of the vacuum-calcined material, analyzed by nitrogen adsorption isotherm data at the end of the calcination process at 540 °C, revealed a smaller surface area and no detectable volume of micropores. A sharp monomodal pore size distribution with a mean value around 108 Å is obtained, larger than the material calcined via the usual procedure, which gives values around 98 Å. The results indicate that the vacuum heat treatment is an alternative calcination strategy for applications which require a well-ordered mesoporous structure, rigid pore walls, and large pore diameters.     

气孔对透明陶瓷激光输出性能的影响

定量分析气孔大小和气孔率对陶瓷激光输出性能的影响,建立了气孔分布模型并结合Mie散射和固体激光技术相关理论,讨论气孔散射对陶瓷激光透过率和输出性能的影响。结果表明,气孔率对激光陶瓷的透过率和斜率效率有着决定性的影响。在给定的气孔尺寸分布下,气孔率越高,陶瓷透过率和激光斜率效率越低;在给定的气孔率下,气孔中心尺寸越大,陶瓷样品的透过率和激光斜率效率越低。减小气孔尺寸至0.3 m以下能有效提高激光斜率效率。气孔越大,激光阈值随气孔率增大而上升越快,越不利于实现激光输出。在实际工作中,改进和控制工艺减小气孔尺寸对提高陶瓷的输出性能同样有着重要意义。     

Characterizing the Evolution of Porosity during Controlled Drug Release

Nuclear magnetic resonance (NMR) techniques have been successfully used to characterize the evolving pore structure of partially soluble pharmaceutical pellets as they absorb water and release soluble components. The restricted diffusivity of water trapped within pellets, which have been immersed in water for differing times, has been measured by pulsed field gradient NMR. These measurements have been used to calculate the surface-to-volume ratio and tortuosity of the pore structure. A one-shot Carr–Purcell–Meiboom–Gill sequence has been used to measure the spin–spin (T ₂) relaxation time of water trapped within the pellets. These data have been regularized and then analyzed by the Brownstein–Tarr model to provide a pore size distribution for the pellets as a function of increasing immersion time. It has been found that pore structure changes significantly as water enters the pellet matrix. Two pellet formulations (herein referred to as placebo and drug-loaded) were studied and showed the same trends of a decreasing surface-to-volume ratio and tortuosity with increasing immersion time. At an immersion time of 10 min, both of these parameters decreased to approximately 70% of their values compared to an immersion time of 2 min. The placebo material tested consistently had both a higher tortuosity and surface-to-volume ratio than the drug-loaded material. At an immersion time of 2 min, the tortuosity for the placebo and drug-loaded materials were about 18 and about 10, respectively, and surface-to-volume ratios of about 6 μm⁻¹ and about 5 μm⁻¹, respectively. The materials tested also show changes in their pore size distribution with immersion time. In both formulations the mean and modal pore sizes increase with immersion time. The placebo material maintains an approximately similar mean and modal pore size, about 2 μm over the timescales studied, suggesting a more symmetric pore size distribution. In the drug-loaded pellets the mean pore size is much higher than the modal pore size, their values being 6.5 and 2.1 μm after 10 min immersion time, respectively. Authors' address: Michael D. Mantle, Department of Chemical Engineering, University of Cambridge, Pembroke Street, Cambridge CB2 3RA, UK     

Adsorption characterization of surfactant-templated ordered mesoporous silicas synthesized with and without hydrothermal treatment

This work reports a systematic study of ordered mesoporous silicas (OMSs) synthesized with and without hydrothermal treatment at 373 K for a series of surfactants of different alkyl chain length (from C10 to C18). For these samples nitrogen adsorption and small angle X-ray scattering (SAXS) data were measured to characterize their adsorption and surface properties. Namely, nitrogen adsorption isotherms were used to evaluate their specific surface area, pore volume and pore size distribution, whereas SAXS data provided information about their structural ordering. It is shown that while the room temperature synthesis afforded OMS samples with cubic MCM-48 structure, an additional 5-day hydrothermal treatment of these samples at 373 K caused their transformation to MCM-41 (two-dimensional hexagonal structure) and improved their pore uniformity, which was manifested by reducing the width of pore size distribution.     

Effects of activated carbon properties on the adsorption of naphthalene from aqueous solutions

The aim of this work was to investigate the role of porous and chemical heterogeneities of activated carbons in the adsorption of naphthalene from aqueous media. A commercially available activated carbon was used as the adsorbent, and its surface heterogeneity was systematically altered by heat treatment at 450 and 850 °C, obtaining a series of carbons with various oxygen contents and similar surface functionalities. The results confirmed that the adsorption of naphthalene depends strongly on the pore size distribution of the adsorbent, particularly narrow microporosity. Moreover, oxygen functionalities reduced the accessibility and affinity of naphthalene to the inner pore structure via formation of hydration clusters. Consequently, the hydrophobic/hydrophilic character of the adsorbent is important, since it dominates the competitive adsorption of water. Adsorbents with a high non-polar character (i.e., low oxygen content) have proven to be more efficient for naphthalene adsorption.     

Pore Structure Analysis of Porous Particles by Modelless and Micropore Method

The modelless (ML) and micropore (MP) methods for the pore structure analysis of porous particles have been studied. Concerning the ML method, it has been shown that the Kiselev equation can only be used to describe condensation and evaporation in capillaries, but cannot be used to describe the increase and decrease of the thickness of the adsorption layer. Strictly speaking, therefore, the ML method is not modelless even for the pore core size distribution. A comparison between the ML method and methods using an equivalent pore model is given. The results of using the ML method in conjunction with a certain pore model are little less accurate than those obtained by adopting the equivalent pore model straightaway. The parameters required for the calculation of both the pore core size and the pore size distribution as well as the conversion between these two calculations are given. Concerning the MP method, it has been shown that the three types of v-t curves, the theoretical foundation of the MP method, are not in one to one correspondance to the three kinds of adsorption mechanism. From the viewpoint of accuracy, the MP method has no advantage over the methods which are based on the condensation mechanism, both have their own merits.     

Influence of initial pH on the particle size and fluorescence properties of the nano scale Eu(III) doped yttria

Europium doped ytrrium oxide (Eu:Y₂O₃) was synthesized by a chemical wet method in the presence of tween-80 and ?-caprolactam in pH range 4-10. It has been observed that the variation in surface area, pore size, and pore volume of the final product, was strongly dependent on the initial pH of the solution. The powder with a large surface area (∼230 m²/g) and low pore diameter (∼16 nm) was obtained when the powder was processed at pH ∼4. The crystallite sizes of the powders processed at pH ∼4 and 10, were found to be 35 and 198 nm, respectively. The structural, chemical and thermal studies of the powders were characterized by X-ray diffraction (XRD), Fourier transformed infrared spectrophotometer (FTIR), Carbon analyzer and Thermogravimetry (TGA). High resolution transmission electron microscopic (HRTEM) study of heat treated powders showed a polygonal morphology with particle size of 40 nm when powder was derived at pH ∼4. Observations of fluorescence suggested that the ⁵D₀→⁷F₂ transition within europium was found to be highly dependent on the initial pH.     

Crystallization of carboxylic acids as studied by NMR Spectrometry

The temperature dependences of the narrow ¹H NMR signals, in the temperature range below phase transition point from the plastic to brittle crystal for pivalic acid (PA) confined in the controlled pore size glasses with mean diameters of 7.9 and 23.9 nm have been investigated in order to determine the depression of the crystallization temperature and the pore size distribution parameters. The obtained parameters and the temperature dependences of the narrow ¹H NMR signals in the solid phases of PA and other carboxylic acids (hexadecanoic (C₁₆), heptadecanoic (C₁₇), octadecanoic (C₁₈), nonadecanoic (C₁₉)) have been used for studying the pore size distributions appeared during the natural crystallization. It was found that the pore size distribution for the even-numbered acids (C₁₆ and C₁₈) is spread over much wider range of the sizes comparing with those for odd-numbered acids (C₁₇ and C₁₉). The maximal value of the pore radius R?=?40.4 nm has been found at the temperature just below the melting point of C₁₈, which is about eight times bigger than that found for C₁₇.     

考虑弥散效应的多孔介质中超绝热燃烧的数值模拟

研究多孔介质内往复流动下的超绝热燃烧。一维模型包括气体输运、多孔介质固体的辐射、导热和气固两相间的对流换热。通过数值计算研究超绝热燃烧的形成、以及弥散效应、当量比和多孔介质材料本身对超绝热燃烧特性的影响。计算结果的有效性通过实验进行了验证并取得了相同的趋势。结果表明,组分弥散效应对气体温度分布和反应热影响很小;同一工况下,不考虑气体混合物的热弥散效应,会导致过高的气体温度计算值。同时,计算结果表明小孔径的多孔介质更有利于贫可燃极限的扩展,对30 ppi的多孔介质燃烧器,得到了当量比为0．092的可燃极限。