Diffusion pore imaging with generalized temporal gradient profiles

In porous material research, one main interest of nuclear magnetic resonance diffusion (NMR) experiments is the determination of the shape of pores. While it has been a longstanding question if this is in principle achievable, it has been shown recently that it is indeed possible to perform NMR-based diffusion pore imaging. In this work we present a generalization of these previous results. We show that the specific temporal gradient profiles that were used so far are not unique as more general temporal diffusion gradient profiles may be used. These temporal gradient profiles may consist of any number of “short” gradient pulses, which fulfil the short-gradient approximation. Additionally, “long” gradient pulses of small amplitude may be present, which can be used to fulfil the rephasing condition for the complete profile. Some exceptions exist. For example, classical q-space gradients consisting of two short gradient pulses of opposite sign cannot be used as the phase information is lost due to the temporal antisymmetry of this profile.     

A facile method to determine pore size distribution in porous scaffold by using image processing

Image processing permits scientists to investigate morphological properties of three-dimensional structures starting from their bi-dimensional gray-scale representation. In many cases porous structure with complex architecture has to be designed in order to attempt specific properties such in the case of scaffold for tissue engineering.Traditional morphological characterization, like scanning electron microscopy, should be coupled with quantitative information such as pore size distribution (PSD) in order to get a deeper understanding of the influence of the porous structure on tissue regeneration processes and on other related applications, it is remarkable to study a quantitative analysis of porosity and of pores dimension.In this work it was developed as a software able to accomplish the segmentation of images containing pores of any geometry in a semi-automatic way with the aim to measure the PSD. Case study constituted by PLA porous scaffolds with different pore size was adopted. Results indicate that image processing methods well fit the pore size features of PLA scaffolds, overcoming the limits of the more invasive porosimetry techniques.     

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.     

Influence of pores on the surface microcompression mechanical response of thermal barrier coatings fabricated by atmospheric plasma spray—Finite element simulation

Surface microcompression is a very important technique to characterize the mechanical properties of film and coating systems. In this paper, surface microcompression simulation for La₂Zr₂O₇ (LZ) thermal barrier coatings (TBCs) was implemented by finite element method, especially, the influence of pores on the surface microcompression mechanical response of the thermal barrier coatings fabricated by atmospheric plasma spray (APS) was focused on. The simulation results indicate that the pores not only affect the stress distribution beneath the contact area between the indenter and coating surface, but also affect the shape of the force-displacement curve and the plastic deformation behavior of TBCs. The micromechanism was discussed in detail in this study. At the same time, by using the surface microcompression technique, a new direction or method was proposed to characterize the pore content of the coating quantitatively.     

Template-free sonochemical synthesis of hierarchically porous NiO microsphere

A novel template-free sonochemical synthesis technique was used to prepare NiO microspheres combined with calcination of NiO_2.45C_0.74N_0.25H_2.90 precursor at 500 °C. The NiO microspheres samples were systematically investigated by the thermograviometric/differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), fourier-transformed infrared spectroscopy (FT-IR), Brunnauer–Emmett–Teller (BET) nitrogen adsorption–desorption isotherms, laser particle size analyzer, and ultraviolet–visible spectroscopy (UV–Vis). The morphology of the precursor was retained even after the calcination process, and exhibited hierarchically porous sphericity. The morphology changed over the ultrasonic radiation time, and the shortest reaction time was 70 min, which was much less than 4 h for the mechanical stirring process. The mechanical stirring was difficult to form the complete hierarchically porous microsphere structure. The BET specific surface area and the median diameter of the hierarchically porous NiO microspheres were 103.20 m²/g and 3.436 μm, respectively. The synthesized NiO microspheres were mesoporous materials with a high fraction of macropores. The pores were resulted from the intergranular accumulation. The ultraviolet absorption spectrum showed a broad emission at the center of 475 nm, and the band gap energy was estimated to be 3.63 eV.     

Densification study of ITO films during high temperature annealing by GISAXS

Three thermal routes were treated on the sol-gel ITO films, i.e. conventional thermal annealing (CTA), rapid thermal annealing (RTA) and thermal cycle annealing (TCA). The near surface and internal structures of films were characterized by grazing incidence small angle X-ray scattering (GISAXS) technique. It is found that slit-like pores show fractal structures laterally and the near surface is sparser with bigger pores. Ordered pore structure normal to the film appears when films are annealed at high heating rate. The shrinkage of pores is mainly owing to structural relaxation and diffusion during the superheating process. However, the supercooling process has no significant effect on the structures. Furthermore, CTA samples have the greatest porosity and surface roughness due to the prevailing crystallization as well as the coarsening procedure. However small pores inside the films are eliminated at low temperature.     

Surface fractal analysis of pore structure of high-volume fly-ash cement pastes

The surface fractal dimensions of high-volume fly-ash cement pastes are evaluated for their hardening processes on the basis of mercury intrusion porosimetry (MIP) data. Two surface fractal models are retained: Neimark's model with cylindrical pore hypothesis and Zhang's model without pore geometry assumption. From both models, the logarithm plots exhibit the scale-dependent fractal properties and three distinct fractal regions (I, II, III) are identified for the pore structures. For regions I and III, corresponding to the large (capillary) and small (C-S-H inter-granular) pore ranges respectively, the pore structure shows strong fractal property and the fractal dimensions are evaluated as 2.592-2.965 by Neimark's model and 2.487-2.695 by Zhang's model. The fractal dimension of region I increases with w/b ratio and hardening age but decreases with fly-ash content by its physical filling effect; the fractal dimension of region III does not evolve much with these factors. The region II of pore size range, corresponding to small capillary pores, turns out to be a transition region and show no clear fractal properties. The range of this region is much influenced by fly-ash content in the pastes. Finally, the correlation between the obtained fractal dimensions and pore structure evolution is discussed in depth.     

Grand canonical Monte Carlo simulation of isotherm for hydrogen adsorption on nanoporous siliceous zeolites at room temperature

Zeolites belong to a most prominent class of nanoporous materials which have been considered as potential sorbents for hydrogen storage. The adsorption of hydrogen molecules on purely siliceous zeolites such as ACO, MEP, ASV, ANA, RWY, and RHO, which encompass a range of different pore structures and their chemical compositions has been simulated employing Grand Canonical Monte Carlo (GCMC) procedure for a temperature range of 250-325 K, and a pressure range of 0-10 kbar. The effects of pore structure of zeolites, temperature and pressure on the hydrogen adsorption has been examined. The results clearly show that the number of adsorbed hydrogen molecules at high pressure, only depends on pore diameter, and the temperature effect on the adsorption decreases with decrease in the number of adsorbed of hydrogen molecules.     

Study on the silica hollow spheres by experiment and molecular simulation

This paper presents the synthesis, characterization and molecular simulation of the silica hollow spheres (SHSs). The SHSs have been prepared using a double-template method, in which the calcium carbonate nanoparticles (CaCO₃) serve as core templates and the cetyltrimethyl-ammonium bromide (CTAB) as wall structure-directing agents. The TEM, XRD, and nitrogen adsorption have been employed to characterize morphologies and structures of the SHSs. The experimental results indicate that the as-prepared sample has an average external diameter of about 85 nm and has occurrence of disordered mesopores in the walls. In the simulation, the SHSs have been modeled as cylindrical pore with pore size distribution according to the experimental data. A combined method of grand canonical Monte Carlo (GCMC) simulation and statistics integral equation (SIE) has been carried out to determine the pore size distribution (PSD) of the SHSs based on the experimental adsorption data of nitrogen at 77 K. The results show that the PSD simulated data are in a good agreement with the experiment, which means that the proposed model for the SHSs is reliable and the combined method of GCMC and SIE is powerful for evaluation of the PSD of the silica hollow spheres.