Blended pastes of cement and lime: Pore structure and capillary porosity

Microstructure of blended pastes of lime and cement were studied in this paper. An increment of complexity of the microstructure was found when pastes increase their percentage in cement. Microstructural characteristics as porosity, morphology of the pores, pore size distribution and surface fractal dimension were evaluated in the different pastes studying the modification with the variation of composition. The capillary water absorption is also evaluated obtaining higher capillary coefficients values for the pastes with higher amounts of lime. The increase of complexity of the microstructure, due to the cement in the pastes, leads to slight deviations of the parallel tube model.     

Effect of drying technique on the physicochemical properties of sodium silicate-based mesoporous precipitated silica

The conventional drying (oven drying) method used for the preparation of precipitated mesoporous silica with low surface area (>300 m²/g) and small pore volume is often associated with a high production cost and a time consuming process. Therefore, the main goal of this study was to develop a cost-effective and fast drying process for the production of precipitated mesoporous silica using inexpensive industrial grade sodium silicate and spray drying of the precipitated wet-gel silica slurry. The precipitated wet-gel silica slurry was prepared from an aqueous sodium silicate solution through the drop-wise addition of sulfuric acid. Mesoporous precipitated silica powder was prepared by drying the wet-gel slurry with different drying techniques. The effects of the oven drying (OD), microwave drying (MD), and spray drying (SD) techniques on the physical (oil, water absorption, and tapping density), and textural properties (specific BET surface area, pore volume, pore size, and % porosity) of the precipitated mesoporous silica powder were studied. The dried precipitated mesoporous silica powders were characterized with field-emission scanning electron microscopy; Brunauer, Emmett and Teller and BJH nitrogen gas adsorption/desorption methods; Fourier-transform infrared spectroscopy; thermogravimetric and differential analysis; N₂ physisorption isotherm; pore size distribution and particle size analysis. There was a significant effect of drying technique on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the mesoporous silica powder. Additionally, the effect of the microwave-drying period on the physicochemical properties of the precipitated mesoporous silica powder was investigated and discussed.     

Porous metal absorbers for underwater sound

Rubber has traditionally been used for underwater sound absorption. Porous metal is a relatively lightweight material and also has higher strength than rubber. However, exactly how porous metals can be used as effective underwater sound absorbers remains unclear. This paper shows how to use porous metal absorbers so that they work well under water, even under fairly constrained conditions. A method of nondimensional analysis is proposed that allows identification of vital characteristics. This means that such characteristics can be varied and the absorbers themselves filled with different types of viscous fluids. Such analysis suggests that the sound absorption coefficient of porous metals does not always increase when there are either increases in porosity or decreases in average pore size. The same method of analysis can show how, by choice of the right characteristics to choose a suitable viscous fluid, a porous metal absorber can be built that takes up little space but still effectively absorbs underwater sounds at low frequencies.     

Influence of porosity on artificial deterioration of marble and limestone by heating

Testing of stone consolidants to be used on-site, as well as research on new consolidating products, requires suitable stone samples, with deteriorated but still uniform and controllable characteristics. Therefore, a new methodology to artificially deteriorate stone samples by heating, exploiting the anisotropic thermal deformation of calcite crystals, has recently been proposed. In this study, the heating effects on a variety of lithotypes was evaluated and the influence of porosity in determining the actual heating effectiveness was specifically investigated. One marble and four limestones, having comparable calcite amounts but very different porosity, were heated at 400 °C for 1 hour. A systematic comparison between porosity, pore size distribution, water absorption, sorptivity and ultrasonic pulse velocity of unheated and heated samples was performed. The results of the study show that the initial stone porosity plays a very important role, as the modifications in microstructural, physical and mechanical properties are way less pronounced for increasing porosity. Heating was thus confirmed as a very promising artificial deterioration method, whose effectiveness in producing alterations that suitably resemble those actually experienced in the field depends on the initial porosity of the stone to be treated.     

Firing-Induced Microstructural Properties of Quasi-Diamagnetic Carbonate-Based Porous Ceramics: a <Superscript>1</Superscript>H NMR Relaxation Correlation Study

This study deals with the application of two-dimensional proton nuclear magnetic resonance relaxometry (2D ¹H NMR-R) to the characterization of porous ceramics nearly free of magnetic compounds. Different microstructural properties were obtained by firing a diamagnetic mixture of kaolin, calcium, and magnesium carbonate over a wide range of maximum temperatures (600–1100 °C) and firing times at the maximum temperature (soaking times) (0–10 h). The 2D ¹H NMR-R method relies on the correlated measurement of ¹H longitudinal (T ₁) and transverse (T ₂) relaxation times of pore-filling water by which the properties of the interconnected pore space may be investigated. In the absence of significant magnetic susceptibility effect due to para- and ferro-magnetic compounds, the 2D ¹H NMR-R maps allow studying the conjoint effects on pore size distribution and inter-pore coupling due to the variations in both time and temperature of firing. The NMR experiments were performed with a low-field ¹H NMR sensor, which allows non-destructive and in situ analysis. For ceramic specimens fired at 600 and 700 °C, the fraction of smallest pores increases with firing time at the expenses of those with intermediate size. The pore shrinkage occurring at this stage, and likely associated with the transformation of kaolinite in metakaolinite, is affected in a similar way by soaking time and firing temperature, in line with the concept of equivalent firing temperature. At temperatures from 800 to 1100 °C, the structural modifications involving interconnectivity and average pore size are driven primarily by firing temperature and, secondarily, by soaking time. The 2D ¹H NMR-R results are confirmed by more traditional, but destructive, mineralogical, and structural analyses like X-ray powder diffraction, helium pycnometry, mercury intrusion porosimetry, and nitrogen adsorption/desorption method.     

Ultrasonic waves in porous ceramics with non-spherical holes

Formulae describing the effective elastic moduli of a porous ceramic medium are derived using Eshelby's solution and Maxwell's approximation. The ceramic medium is considered as an infinite matrix, which has uniform elastic properties and encloses non-spherical pores. A numerical evaluation of the velocity of an ultrasonic wave in the ceramic, as function of the porosity and pore shape, is presented. The theoretical results were combined with those obtained experimentally for different firing temperatures of the ceramic.     

Lime-pastes with different kneading water: Pore structure and capillary porosity

Lime-mortars to be used in restoration works of Cultural Heritage are being more and more studied. The knowledge on the lime-pastes allows understanding the behaviour of the binder fraction. The aim of this work is to study the influence of the kneading water on two critical aspects of the lime-pastes: pore structure and capillary porosity, because both of them are related to the service life of the material, particularly with the moisture transport. Mercury intrusion porosimetry has been performed to establish the pore size distribution: one pore range has been checked in the different pastes tested, setting linear relationships between the pore diameter and the water/lime ratio.Fractal geometry has been used from the MIP results in order to evaluate the pore surface complexity, as a function of the kneading water. From the results, it can be concluded that kneading water is only responsible for a swelling of the structure, but it does not change the pore surface (keeping constant the surface fractal dimension). DIA analysis has been carried out, confirming the previous results. Finally, the correlation obtained between the capillary coefficient and the water/lime ratio confirms the postulated pore structure for the different amount of kneading water in lime-pastes.     

Salt crystallization as damage mechanism in porous building materials--a nuclear magnetic resonance study

Salts can damage building materials by chemical reactions or crystallization, which is a serious threat to cultural heritage. In order to develop better conservation techniques, more knowledge of the crystallization processes is needed. In a porous material, the size of a salt crystal is limited by the sizes of the pores. It has been predicted that as a consequence, the solubility of a salt increases with decreasing pore size. This increase seems to be related to an increase of the stress generated by a crystal on the pore wall. It has been suggested that the resulting stress could become high enough to induce failure. We have studied the crystallization of salts in porous materials with well-defined pore sizes. Samples were saturated at 40 degrees C with saturated Na2SO4 and Na2CO3 solutions. Next we have cooled the samples to 0 degrees C and waited for nucleation. After nucleation occurred, the solubility in the porous material was measured with nuclear magnetic resonance (NMR) as a function of the temperature. The measurements on Na2CO3 indeed show an increase in solubility with a decrease in pore size. For Na2SO4, we did not observe a pore size-dependent solubility. However, we have to remark that these results show a metastable crystal phase. The results can be used to calculate the actual pressure exerted by the crystals onto the pore wall.     

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.     

Improvement of sintering,nonlinear electrical,and dielectric properties of ZnO-based varistors doped with TiO_2

The effects of TiO_2 on sintering and nonlinear electrical properties of(98.5-x)ZnO–0.5MnO_2–0.5Co_2O_3-0.5Bi_2O_(3–x)TiO_2(x = 0.3,0.5,0.7,0.9 mol%) ceramic varistors prepared by the ceramic technique are investigated in this work.The optimum sintering temperature of the prepared samples is deduced by determining the firing shrinkage and water absorption percentages.The optimum sintering temperature is found to be 1200℃,at which each of the samples shows a maximum firing shrinkage and minimum water absorption.Also minimum water absorption appears in a sample of x = 0.9 mol%.Higher sintering temperature and longer sintering time give rise to a reduction in bulk density due to the increased amount of porosity between the large grains of ZnO resulting from the rapid grain growth induced by the liquid phase sintering.The crystal size of ZnO decreases with increasing TiO_2 doping.The addition of TiO_2 improves the nonlinear coefficient and attains its maximum value at x = 0.7 mol% of TiO_2,further addition negatively affects it.A decrease in capacitance consequently in the dielectric constant is recorded with increasing the frequency in a range of 30 kHz–200 kHz.The temperature and composition dependences of the dielectric constant and AC conductivity are also studied.The increase of temperature raises the dielectric constant because it increases ionic response to the field at any particular frequency.     

光栅图像传输法测量海水光学传递函数

根据成像系统光学传递函数的相乘率,用刻有不同空间频率光栅的目标板,研究了在有水体和无水体情况下,光栅图像的传输情况。然后运用mathcad2001软件对采集到的光栅图像进行分析和计算,获得海水的光学传递函数。通过人为地改变水体长度、水中悬浮物质浓度和水体含盐量等,定性地研究了影响海水光学传递函数的因素。该测量方法在激光水下成像、水下目标探测以及对潜激光通信都将具有重要的推广应用价值。     

Water absorption kinetics in different wettability conditions studied at pore and sample scales in porous media by NMR with portable single-sided and laboratory imaging devices

NMR relaxation time distributions of water (1)H obtained by a portable single-sided surface device have been compared with MRI internal images obtained with a laboratory imaging apparatus on the same biocalcarenite (Lecce Stone) samples during capillary water uptake. The aim of this work was to check the ability of NMR methods to quantitatively follow the absorption phenomenon under different wettability conditions of the internal pore surfaces. Stone wettability changes were obtained by capillary absorption of a chloroform solution of Paraloid PB72, a hydrophobic acrylic resin frequently used to protect monuments and buildings, through one face of each sample. Both relaxation and imaging data have been found in good quantitative agreement each other and with masses of water determined by weighing the samples. In particular the Washburn model of water capillary rise applied to the imaging data allowed us to quantify the sorptivity in both treated and untreated samples. Combining relaxation and imaging data, a synergetic improvement of our understanding of the water absorption kinetics at both pore and sample scales is obtained. Since relaxation data have been taken over the course of time without interrupting the absorption process, simply by keeping the portable device on the surface opposite to the absorption, the results show that the single-sided NMR technique is a powerful tool for in situ evaluation of water-repellent treatments frequently used for consolidation and/or protection of stone artifacts.     

Nano-pore size and porosity study by means of Nuclear Magnetic Resonance and Positronium Annihilation Lifetime

The present work involves a comprehensive experimental determination of porosity and pore size distribution in rocks from oil fields formations by deuterium (²H) Nuclear Magnetic Resonance (NMR) and Positronium Annihilation Lifetime Spectroscopy (PALS). Both techniques yield complementary results; PALS measures the average pore size providing bulk information from which the most abundant pore size can be obtained, and NMR allows for the determination of the relative pore size distribution accurately. Both techniques give complementary information to obtain an absolute pore size distribution.     

Characterization of partially sintered ceramic powder compacts using fluorinated gas NMR imaging.

We use nuclear magnetic resonance (NMR) imaging of C2F6 gas to characterize porosity, mean pore size, and permeability of partially sintered ceramic (Y-TZP Yttria-stabilized tetragonal-zirconia polycrystal) samples. Conventional measurements of these parameters gave porosity values from 0.18 to 0.4, mean pore sizes from 10 nm to 40 nm, and permeability from 4 nm(2) to 25 nm(2). The NMR methods are based on relaxation time measurements (T(1)) and the time dependent diffusion coefficient D(Delta). The relaxation time of C2F6 gas is longer in pores than in bulk gas and it increases as the pore sizes decrease. NMR yielded accurate porosity values after correcting for surface adsorption effects. A model for T(1) dependence on pore size that accounts for collisions between gas molecules and walls as well as surface adsorption effects is proposed. The model fits the experimental data well. Finally, the long time limit of D(Delta)/D(o), where D(o) is the bulk gas diffusion coefficient is useful for measuring tortuosity, while the short time limit was not achieved experimentally and could not be used for calculating surface-area to volume (S/V) ratios.     

凤阳明中都遗址出土琉璃瓦胎体制作工艺研究

为探索明代初期中国琉璃瓦制作工艺技术水平与工艺特点,运用能量色散X射线荧光光谱法（energy disperse X-ray fluorescence, EDXRF）,对安徽凤阳明中都及南京明故宫遗址出土69件琉璃瓦样品胎体化学组成进行了测定,同时利用热膨胀仪、吸水率测定仪和偏光显微镜等仪器设备对样品胎体的烧成温度、吸水率、显气孔率、体积密度与显微结构等进行了分析。分析结果显示,明中都样品胎体根据元素化学组成差异可分为高钙高铁、低钙高铁和低钙低铁三种类型,表明该遗址琉璃瓦样品胎体制作原料可能具有不同来源,同时,部分明中都样品的化学组成与南京明故宫样品较为接近,而上述两处遗址样品与北京故宫样品在化学组成上皆具有显著差异。烧成温度、物理性能和显微结构分析结果显示,明中都琉璃瓦瓷质胎体样品的烧成温度较高,达到了1 141 ℃,且吸水率和显气孔率明显较低,达到了瓷胎的标准,而陶质胎体琉璃瓦样品的烧成温度约为880~1 100 ℃,吸水率和显气孔率较大,且不同样品间差异明显,这可能是由于明中都琉璃瓦胎体的来源不同,导致不同样品在烧成温度、吸水率、显气孔率等方面差异较大。与北京、南京二处的琉璃瓦样品相比,明中都样品吸水率及显气孔率稍微高于二处,但三处陶胎琉璃瓦样品胎体的烧成温度基本都在1 100 ℃以下。明中都三种不同类型样品胎体显微结构差异较小,矿物颗粒粒径和孔隙大小相近,其中部分石英晶体具有明显的熔蚀边。此外,明中都和明故宫样品的显微结构特点显示两处遗址样品胎体原料加工皆较为精细,原料淘洗和烧结程度较高,琉璃瓦物理性能较好。对明初洪武时期明中都出土琉璃瓦烧制工艺的研究结果,不仅可为了解我国琉璃瓦工艺发展历程、还可对探索明初琉璃制作工艺和明中都营建的组织形式等提供科学依据。     

Sound absorption of cellular metals with semiopen cells

A combined experimental and theoretical study is presented for the feasibility of using aluminum foams with semiopen cells for sound-absorption applications. The foams are processed via negative-pressure infiltration, using a preform consisting of water-soluble spherical particles. An analytical model is developed to quantify the dependence of pore connectivity on processing parameters, including infiltration pressure, particle size, wetting angle, and surface tension of molten alloy. Normal sound-absorption coefficient and static flow resistance are measured for samples having different porosity, pore size, and pore opening. A theory is developed for idealized semiopen metallic foams, with a regular hexagonal hollow prism having one circular aperture on each of its eight surfaces as the unit cell. The theory is built upon the acoustic impedance of the circular apertures (orifices) and cylindrical cavities due to viscous effects, and the principle of electroacoustic analogy. The predicted sound-absorption coefficients are compared with those measured. To help select processing parameters for producing semiopen metallic foams with desirable sound-absorbing properties, emphasis is placed on revealing the correlation between sound absorption and morphological parameters such as pore size, pore opening, and porosity.     

Time domain dispersion of underwater optical wireless communication

A new method to count the expected value and variance of time dispersion is presented for time dispersion of underwater optical wireless communication.Instead of the typically used Gamma distribution,inverseGaussian distribution is suggested for underwater optical impulse response time waveform function.The expectation of this method is in good agreement with experimental data.Future works may include water absorption to the model.     

Pore size assessment based on wall collision broadening of spectral lines of confined gas: experiments on strongly scattering nanoporous ceramics with fine-tuned pore sizes

Wall collision broadening of absorption lines of gases confined in porous media is a recently opened domain of high-resolution spectroscopy. Here, we present an experimental investigation of its application for pore size assessment. We report on the manufacturing of nanoporous zirconia ceramics with well-defined pore sizes fine-tuned from 50 to 150 nm. The resulting pore structure is characterized using mercury intrusion porosimetry, and the optical properties of these strongly scattering materials are measured using femtosecond photon time-of-flight spectroscopy (transport mean free paths found to be tuned from 2.3 to 1.2 μm as the pore size increase). Wall collision line broadening is studied by performing near-infrared (760 nm) high-resolution diode laser spectroscopy of confined oxygen molecules. A simple method for quantitative estimation of the pore size is outlined and shown to produce results in agreement with mercury intrusion porosimetry. At the same time, the need for improved understanding of wall collision broadening is emphasized.     

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.     

Understanding compressive deformation in porous titanium

The aim of this study was to understand and compare the compression deformation behavior of porous metals with random and designed porosity. Direct observation, analysis and quantification of porosity parameters using microcomputed tomography (µCT) enabled the determination of relationship between porosity characteristics and compressive deformation of porous titanium. Porosity and pore size variations before and after deformation showed relatively uniform deformation in the sample with random porosity compared to designed porosity. Strong, continuous and regular arrangement of load-bearing sections in the designed porosity sample imparted higher Young's modulus and 0.2% proof strength than for the random porosity sample. The experimental results clearly showed the dependence of deformation behavior and mechanical properties on pore distribution and continuity of load-bearing cross-section.