Effect of Silica Fume on Metakaolin Geopolymers' Sulfuric Acid Resistance.

To demonstrate the importance of the Si/Al ratio in terms of geopolymer mix designs for acid resistance, a metakaolin-based geopolymer was modified by replacing the aforementioned precursor with different percentages of silica fume. Durability tests were performed by exposing geopolymers with varying amounts of silica fume (up to 9%) to sulfuric acid solution (pH 1) over a period of 84 days. Geopolymer samples were analyzed by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) before and after 7, 14, 28, 56 and 84 days of exposure. To show the time-dependent change of the elemental composition in the corroded layer after sulfuric acid attack, SEM-EDX elemental mappings were conducted and divided into 100 µm segments to generate element-specific depth profiles. The results show that above a critical silica fume content, the erosion of the sample surface by complete dissolution can be prevented and higher amounts of silica fume lead to a significant densification of large (protective) areas of the corroded layer, which delays the progress of corrosion.

Electrochemical growth mechanism of nanoporous platinum layers.

Porous platinum is a frequently used catalyst material in electrosynthesis and a robust broadband absorber in thermoelectrics. Pore size distribution and localization determine its properties by a large extent. However, the pore formation mechanism during the growth of the material remains unclear. In this work we elucidate the mechanism underlying electrochemical growth of nanoporous platinum layers and its control by ionic concentration and current density during electrolysis. The electrode kinetics and reduction steps of PtCl4 on platinum electrodes are investigated by cyclic voltammetry and impedance measurements. Cyclic voltammograms show three reduction steps: two steps relate to the platinum cation reduction, and one step relates to the hydrogen reduction. Hydrogen is not involved in the reduction of PtCl4, however it enables the formation of nanopores in the layers. These findings contribute to the understanding of electrochemical growth of nanoporous platinum layers in isopropanol with thickness of 100 nm to 500 nm.

Evaluation of Sulfuric Acid-Induced Degradation of Potassium Silicate Activated Metakaolin Geopolymers by Semi-Quantitative SEM-EDX Analysis.

Geopolymers are synthesized by mixing powdery solids, rich in amorphous silicon and aluminum species, with an alkaline solution, which leads to the formation of an inorganic alumosilicate network. Their acid resistance is affected by the composition, the porosity, and pore size distribution of the hardened binder as well as the type and concentration of the acidic solution. In the present study, two geopolymer mixtures with varying liquid-to-solid ratios and Si/Al ratios were exposed to a sulfuric acid solution (pH = 1) and analyzed after different durations of exposure (7, 14, 28, 56, and 70 days) by using a light microscope and scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX). SEM-EDX elemental mapping was used to evaluate the degradation from depth profiles of silicon (Si), aluminum (Al), and potassium (K) leaching. The results clearly show the leaching kinetics of potassium and the dealumination of the network. The separate consideration of specific reaction steps in the course of degradation, namely the depth of erosion (DE), the depth of deterioration (DD), and the depth of reaction for certain elements (DR(e)), indicate a combination of chemical and diffusion controlled degradation mechanisms.

Reactivity and Microstructure of Metakaolin Based Geopolymers: Effect of Fly Ash and Liquid/Solid Contents.

Geopolymers are inorganic binders based on mixtures of an aluminosilicate powder with an alkali-silicate solution. Properties of geopolymers are strongly determined by the type of reactive solid, the liquid/solid ratio of paste and, amongst others, the Si/Al ratio of the formed geopolymer network. In this study, fly ash blended metakaolin based geopolymers with varying liquid/solid ratios (l/s), activated by potassium silicate solution, are investigated. Reactivity of metakaolin and fly ash was investigated by powder X-ray diffraction (XRD) and dissolution tests. Reactivity, mechanical properties and microstructure of hardened pastes were analyzed by setting and compressive strength tests, mercury intrusion porosimetry (MIP), capillary water absorption tests, thermogravimetric analysis-differential scanning calorimeter (TGA-DSC), isothermal calorimetry and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). The results show that substitution of metakaolin by fly ash as well as variation of l/s brings advantages up to a certain degree, but also has a considerable influence on the pore size distribution, mechanical properties, Si/Al ratio of the geopolymer network and the content of bound water.

Geopolymer, Calcium Aluminate, and Portland Cement-Based Mortars: Comparing Degradation Using Acetic Acid.

In this paper, we comparitvley studied acetic acid attacks on geopolymer (GP-M), calcium aluminate (CAC-M), and Portland cement (PC-M)-based mortars. Consequent formations of deteriorated or transition layers surrounding the unaltered core material was classified in these three mortars, according to different degradation levels depending on what binder type was involved. Apart from mass loss, hardness, and deterioration depth, their microstructural alterations were analyzed using test methods such as scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS), mercury intrusion porosimetry (MIP), powder X-ray diffraction (XRD), and thermogravimetric analysis-differential scanning calorimeter (TGA-DSC), which showed the different mechanisms for each binder type. Elemental maps revealed the decalcification (PC-M and CAC-M) and depolymerization (GP-M) that occurred across the mortar sections. The mass loss, hardness, and porosity were the least affected for GP-M, followed by CAC-M. These results points out that geopolymer-based mortars have improved acid resistance, which can be used as a potential alternative to conventional cement concretes that have been exposed to agro-industrial environments.

A new two-chip concept for continuous measurements on PMMA-microchips.

A new concept for continuous measurements on microchips is presented. A PMMA (polymethylmethacrylate) based capillary electrophoresis chip with integrated conductivity detection is combined with a second chip, which undertakes the task of fluid handling and electrical connections. The combination of electrokinetic and hydrodynamic flows allows long-term continuous stable analyses with good reproducibilities of migration time and peak heights of analytes. The two-chip system is characterized in terms of stability and reproducibility of separation and detection of small ions. Relative standard deviations of <1% and 3% respectively for retention times and peak heights during long-term measurements can be achieved. The new system combines simple handling and automated analysis without the need for refilling, cleaning or removal of the separation chip after one or several measurements.