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Aim of this study is to provide information about moisture dependent material behaviour of unstabilised loadbearing earth blocks and mortars. Compressive strength and Young’s modulus were investigated after conditioning in varying relative humidity reaching from 40 % up to 95 %. The material composition and physical properties were investigated to understand the influence of relative humidity onto the mechanical properties. A normalisation of strength and stiffness by the values obtained at 23 ◦C and 50 % relative humidity reveals a linear dependence of compressive strength and Young’s modulus that is regardless of the material composition.
Thus, it is possible to describe the influence of relative humidity onto the load-bearing behaviour of unstabilised earth masonry materials in a generally valid formulation.
Alkali-silica reaction (ASR) is a chemical reaction within concrete which can lead over time to cracking and spalling. Due to the complexity of the problem, it still causes damage to concrete constructions worldwide.
The publication aims to illustrate the interdisciplinary research of the German Federal Institute for Materials Research and Testing (BAM) within the last 20 years, considering all aspects of ASR topics from the macro to the micro level. First, methods for characterization and assessment of ASR risks and reaction products used at BAM are explained and classified in the international context. Subsequently the added value of the research approach by combining different, preferably nondestructive, methods across all scales is explained using specific examples from a variety of research projects. Aspects covered range from the development of new test-setups to assess aggregate reactivity, to analysis of microstructure and reaction products using microscopical, spectroscopical and X-ray methods, to the development of a testing methodology for existing concrete pavements including in-depth analysis of the visual damage indicator and the de-icing salt input using innovative testing techniques. Finally, research regarding a novel avoidance strategy that makes use of internal hydrophobization of the concrete mix is presented.
If the amount of sulfate within the mix design for concrete is not balanced, ettringite formation which first controls solidification continues while the concrete is hardening. Ettringite forms by reaction of sulfate contained in the cement or in some admixture with calcium aluminate (C3A) as cement component. The “late primary ettringite formation” promotes an increase in volume within the hardened concrete leading to cracks. To analyze the effect of substituting part of ordinary Portland cement (OPC) by a treated brown coal fly ash mortar bars were tested according to ASTM C452. This test method was originally developed to extrapolate from the internal to external sulfate attack and is based on the idea that by testing a concrete mixture containing sulfate the process of deterioration is accelerated because it does not have to diffuse into the concrete before reaction first. In addition to the samples prescribed in ASTM C452 further samples in the size of the German SVA procedure were tested also designed for accessing the external sulfate resistance. The results show that while the replacement of 25 % of cement by brown coal fly ash leads to length changes around the limit defined by ASTM, the substitution of 50 % cement exceeded the limit by a multiple. The progress of expansion is the very similar for the two geometries tested. In-situ XRD measurements confirmed that while for pastes made of OPC the formation of ettringite is completed after 20 hours, this is not true for the mixtures containing the brown coal fly ash.
In a different study the effect of hydrothermal treatment on the phase composition of ultra-high-performance concrete was analyzed. The results show that the sulfate and aluminate resulting from the decomposition of ettringite are bound into new phases.
If this binding is permanent this might allow the larger use of sulfate bearing raw materials.
Basic oxygen furnace slags (BOFS) are by-products of the steelmaking process. Several researchers have studied the production of Portland cement clinker and metallic iron from BOFS via a reductive treatment.
In this study, we applied a carbothermal reduction of BOFS in a technical-scale electric arc furnace and characterised the clinker-like products. Those clinker-like non-metallic products (NMPs) had a chemical and mineralogical composition comparable to clinker for ordinary Portland cement (OPC) and contained large elongated alite crystals as major component. The pure NMPs reacted more slowly and achieved a lower degree of hydration compared with commercial OPC.
If the reactivity of the products can be further increased by employing specific adaptations, it can be used as a full clinker substitute for OPC. Nevertheless, it is also an option to use the material without further modifications as a cement component or concrete addition, which contributes to the strength development in both cases.
Hydrous lithium aluminosilicate (L–A–S–H) and lithium aluminate (L–A–H) gels are candidate precursors for glass-ceramics and ceramics with potential advantages over conventional processing routes. However, their structure before calcination remained largely unknown, despite the importance of precursor structure on the properties of the resulting materials. In the present study, it is demonstrated that L–A–S–H and L–A–H gels with Li/Al ≤ 1 can be produced via an organic steric entrapment route, while higher Li/Al ratios lead to crystallization of gibbsite or nordstrandite. The composition and the structure of the gels was studied by thermogravimetric analysis, X-ray diffraction, 27Al and 29Si magic-angle spinning nuclear magnetic resonance, and Raman spectroscopy. Aluminium was found to be almost exclusively in six-fold coordination in both the L–A–H and the L–A–S–H gels. Silicon in the L–A–S–H gels was mainly in Q4 sites and to a lesser extent in Q3 sites (four-fold coordination with no Si–O–Al bonds). The results thus indicate that silica-rich and aluminium-rich domains formed in these gels.
The oxidation of sulfur in aqueous solutions is an important process in several geochemical and industrial contexts. In concrete technology, it is particularly relevant for the protection of steel reinforcement in slag cement-based concretes, as the presence of sulfides affects the passivation of the steel and corrosion initiation in the presence of chlorides. However, the knowledge about the kinetics of sulfide oxidation in alkaline solutions, such as concrete pore solutions, is incomplete. To address this issue, we prepared solutions with 0.80 M NaOH, and nominally 10, 100 and 350 mM HS−, respectively, and followed the evolution of the sulfur species during bubbling with oxygen-containing gas (concentration 100% or 22%) using X-ray absorption near-edge structure (XANES) spectroscopy at the sulfur K-edge. Polysulfide, thiosulfate, sulfite and sulfate were identified and quantified via linear combination fitting of the spectra, using previously measured standards. A preliminary analysis of the results shows that the initial rate constant of sulfide oxidation depends strongly on the HS− concentration, while it less strongly depending on the oxygen concentration, in line with previous results for lower pH values. Approaches to fit the data to obtain the rate constants of all relevant reactions will be discussed.
Powder X-ray diffraction is a time-consuming and challenging task, especially for preparation of sensitive phases like ettringite and calcium-silicate-hydrate (C-S-H) phases. Fine-grained ultrahigh-performance concrete (UHPC) with an average grain size <100 μm could be investigated directly without time-consuming milling. As a proof of concept, small UHPC cylinders with plain surfaces were investigated with a newly designed sample holder. The comparison with conventionally prepared powder shows the feasibility of fast qualitative phase analysis using this approach. As a great benefit, a depth-dependent analysis, as well as a comparison of surface layers and core material, was carried out.
Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter.
Tricalcium-silicate (C3S) or Alite is the most important mineral in Portland cement. Since pure tricalcium-silicate is only stable above temperatures of 1250 °C, its decomposition has to be prevented technically by fast cooling after the sintering process. At room temperature, the decomposition velocity is very slow so that metastable tricalcium-silicate is obtained.
Although the mechanisms of clinker phase formation during burning process of Portland cement in a rotary kiln were solved and improved over the years, in view of possible economic and ecological benefits current projects aim to produce clinker phases from metallurgical slags. Recent studies discovered that the mineral phase which remained after a reducing treatment and separation of formed metallic iron from molten Linz-Donawitz (LD-) slags contained about 60 wt.% Alite despite it was cooled slowly. Because the results could be verified using slags from different origins and varying cooling velocities a chemical stabilisation of the Alite can be assumed. First tests in mortars indicate that workability, hardening and solid state properties are comparable with an ordinary Portland cement. An application of the observed phenomenon in cement production requires enhanced knowledge about formation and stabilisation conditions of Alite during crystallisation from melts in contrast to the sintering reactions in conventional Portland cement production. Therefore, this study focuses on the stabilisation mechanisms of Alite in consolidating melts. Samples from different melting experiments are analysed to determine stabilising factors.
Tricalcium aluminate (C3A) is found with less than 10% wt. of the total composition; however, during hydration, C3A plays an important role in the early hydration of cement in the presence of gypsum as a set retarder.
The aim of this investigation is to assess the suitability of optical spectroscopy and a dye-based optical probe to monitor early hydration of C3A in the presence of gypsum and hemihydrate. Optical evaluation was performed using steady-state fluorescence and diffuses reflectance spectroscopy (UV-VisDR). Phase characterization during hydration was done with in-situ X-ray diffraction. UV-VisDR with a cyanine dye probe was used to monitor the formation of metastable phases and was employed together with fluorescence spectroscopy, to follow the Aggregation and disaggregation of the dye during hydration. In conclusion, for the first time, a cyanine dye was identified as a feasible and stable probe to monitor C3A hydration changes in the presence of calcium sulfate.