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Paper des Monats
- ja (2)
Diffusional gas transport of a H2/CO2 mixture versus N2 in the pore system of hardened cement pastes was studied at four temperatures up to 350 °C in a Wicke-Kallenbach cell. The pastes possessed separation factors αH2,CO2 from 1.42 to 3.43, i.e. the diffusion of hydrogen took place considerably faster than the diffusion of carbon dioxide. The separation factors depended on the threshold radii of the pastes, smaller threshold radii leading to higher separation factors. The Knudsen numbers of the controlling constrictions of the pore system and the temperature dependence of the effective diffusion coefficients of the gases show that gas transport in these constrictions takes place in the transient regime between Knudsen diffusion and bulk diffusion, smaller constriction widths leading to predominating Knudsen diffusion. It is therefore possible to use cement paste membranes to separate gas components of low molecular weight from higher weight components.
A silica residue from waste treatment of chlorosilane production was used together with solid sodium aluminate to test its applicability for the production of one-part geopolymers. The blend was activated with water and cured at 70 °C. The degree of reaction and strength were determined after 1, 3, and 7 days. The reaction products were analyzed by XRD and SEM/EDX. Until the third day of curing the degree of reaction of the residue reached 51 % and the strength was 8.9 MPa. The reaction product was identified as geopolymer containing zeolite A. Thus, the results confirmed that the residue may be used in the production of geopolymers. However, after 3 days of curing no further progress of reaction was observed and the strength slightly decreased, which was attributed to changes in the structure of the geopolymeric gel. It was further observed that even harsh vacuum drying left some water (presumably zeolitic water and surface hydroxyl groups) in the geopolymer.
The conversion of hydrated calcium aluminate cement (CAC) leads to an increase of its porosity which results in lower strength and higher permeability. Due to particular failures in the past, caused by conversion of CAC concretes, their use is sometimes considered to be not reliable. To evaluate the durability of converted CAC, pastes of two CACs were prepared at low w/c ratios (0.25 and 0.35), heated to 105 °C for 15 days and investigated by means of helium pycnometry, mercury porosimetry and nitrogen adsorption as well as by air permeability measurements. The results were compared to the pore structure properties and permeabilities of hardened Portland cement (OPC) pastes. At identical w/c, CAC pastes and OPC pastes exhibited similar open and total porosities. The threshold radii of the CAC pastes were about one order of magnitude greater while the hydraulic radii of their open pore system were smaller. The CAC pastes possessed somewhat smaller permeabilities than the OPC pastes and can thus be regarded as being as durable as the latter in this respect. From comparison of pore structure parameters and permeabilities it was furthermore concluded that significant pore structure damage occurs in the CAC pastes during mercury porosimetry measurements and therefore the measured threshold radii have to be considered as unreliable.
Reaction products and strength development of wastepaper sludge ash and the influence of alkalis
(2014)
Wastepaper sludge ash (WSA) from a newsprint paper mill was investigated for its mineralogical composition and its reaction products and strength development after activation with water and sodium and potassium hydroxide solutions. The results showed the WSA to consist of calcite, free lime, gehlenite, tricalcium aluminate, belite, talc, quartz and probably a glassy phase. The principle reaction product was monocarboaluminate (CO3–AFm) for the water- as well as for the alkali-activated WSA. Formation of monocarboaluminate and strength gain was more rapid for the alkali-activated WSA until 1 day of curing. However, afterwards reactions proceeded much slower when alkali solutions were used, leading to an about twice as high compressive strength for water-activated WSA mortars after 28 days of curing. The observed behavior is tentatively ascribed to a less uniform microstructure of the alkali-activated WSA. Significant differences between NaOH- and the KOH-activated WSA were not observed.
Gas separation is a key issue in various industrial fields. Hydrogen has the potential for application in clean fuel technologies. Therefore, the separation and purification of hydrogen is an important research subject. CO2 capture and storage have important roles in 'green chemistry'. As an effective clean technology, gas separation using inorganic membranes has attracted much attention in the last several decades. Membrane processes have many applications in the field of gas separation. Cement is one type of inorganic material, with the advantages of a lower cost and a longer lifespan. An experimental setup has been created and improved to measure twenty different cement membranes. The purpose of this work was to investigate the influence of gas molecule properties on the material transport and to explore the influence of operating conditions and membrane composition on separation efficiency. The influences of the above parameters are determined, the best conditions and membrane type are found, it is shown that cementitious material has the ability to separate gas mixtures, and the gas transport mechanism is studied.
Metakaolin-based alkali activated mortars (AAM) - with and without CuSO4·5H2O and ZnO addition (mass ratio Mn+/solid binder 0.08% to 1.7%) - were casted and exposed within an extensive long-term field campaign over the period of 20 months to a sewer basin, strongly affected by biogenic acid corrosion. (Un-)exposed AAM were tested regarding their physicochemical and microstructural properties, bioreceptivity and overall durability. Metal addition led to a retarding effect during alkali-activation reaction, as well as to an increase in open porosity of up to 3.0% and corresponding lower compressive strength of up to 10.9%. Reduced microbial colonization and diversity were observed on AAM with Cu, while Zn addition led to increased biodiversity. We propose that the observed higher durability of Cu-doped AAM is due to antibacterial effects and associated reduction of biogenic acid production, superseding overall negative effects of metal-dosage on physical material properties. Observed lower durability of Zn-doped AAM was related to combined negative physicochemical and microbial effects.
Hybrid cements are composites made of Portland cement or Portland clinker and one or more supplementary cementitious materials like slag, fly ash or metakaolin, activated with an alkali salt. To date, their hydration mechanism and the phase formation at various temperatures is insufficiently understood, partly due to the large variability of the raw materials used. In the present study, three hybrid cements based on ground granulated blast furnace slag, fly ash, Portland clinker and sodium sulfate, and an alkali-activated slag/fly ash blend were cured at 10 and 21.5°C, and subsequently analyzed by XRD, 27Al MAS NMR, and TGA. The compressive strength of the hybrid cements was higher by up to 27% after 91-day curing at 10°C, compared to curing at 21.5°C. The experimental results as well as thermodynamic modeling indicate that the differences in compressive strength were related to a different phase assemblage, mainly differing amounts of strätlingite and C-N-A-S-H, and the associated differences of the volume of hydration products. While the strätlingite was amorphous to X-rays, it could be identified by 27Al MAS NMR spectroscopy, TGA and thermodynamic modeling. The microstructural properties of the hybrid cements and the alkali-activated slag/fly ash blend as well as the compatibility between thermodynamic modeling results and experimental data as a function of curing temperature and time are discussed.
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 current understanding of the carbonation and the prediction of the carbonation rate of alkali-activated concretes is complicated inter alia by the wide range of binder chemistries used and testing conditions adopted. To overcome some of the limitations of individual studies and to identify general correlations between mix design parameters and carbonation resistance, the RILEM TC 281-CCC ‘Carbonation of Concrete with Supplementary Cementitious Materials’ Working Group 6 compiled and analysed carbonation data for alkali-activated concretes and mortars from the literature. For comparison purposes, data for blended Portland cement-based concretes with a high percentage of SCMs (≥ 66% of the binder) were also included in the database. The analysis indicates that water/CaO ratio and water/binder ratio exert an influence on the carbonation resistance of alkali-activated concretes; however, these parameters are not good indicators of the carbonation resistance when considered individually. A better indicator of the carbonation resistance of alkali-activated concretes under conditions approximating natural carbonation appears to be their water/(CaO + MgOeq + Na2Oeq + K2Oeq) ratio, where the subscript ‘eq’ indicates an equivalent amount based on molar masses. Nevertheless, this ratio can serve as approximate indicator at best, as other parameters also affect the carbonation resistance of alkali-activated concretes. In addition, the analysis of the database points to peculiarities of accelerated tests using elevated CO2 concentrations for low-Ca alkali-activated concretes, indicating that even at the relatively modest concentration of 1% CO2, accelerated testing may lead to inaccurate predictions of the carbonation resistance under natural exposure conditions.
The current understanding of the carbonation of alkali-activated concretes is ham-pered inter alia by the wide range of binder chemistries used. To overcome some of the limitations of individual studies and to identify general correlations between their mix design parameters and carbonation resistance, the RILEM TC 281-CCC working group 6 compiled carbonation data for alkali-activated concretes and mortars from the literature. For comparison purposes, data for blended Portland cement-based concretes with a high percentage of SCMs (≥ 66 % of the binder) were also included in the database. A preliminary analysis of the database indicates that w/CaO ratio and w/b ratio exert an influence on the carbonation resistance of alkali-activated concretes but, contrary to what has been reported for concretes based on (blended) Portland cements, these are not good indicators of their carbonation resistance when considered individually. A better indicator of the carbonation resistance of alkali-activated concretes under conditions approxi-mating natural carbonation appears to be their w/(CaO + Na2O + K2O) ratio. Furthermore, the analysis points to significant shortcomings of tests at elevated CO2 concentrations for low-Ca alkali-activated concretes, indicating that even at a concentration of 1 % CO2, the outcomes may lead to inaccurate predictions of the carbonation coefficient under natural exposure conditions.
One-part geopolymers offer advantages over conventional geopolymers with regard to handling and storage of feedstocks. However, they often suffer from a low degree of reaction, a high amount of crystalline byproducts, and consequently low strength. In this study, one-part geopolymers were produced from rice husk ash (RHA) and sodium aluminate, and investigated by XRD, ATR-FTIR, SEM and compressive strength testing. The compressive strength of the material was 30 MPa, i.e. significantly higher than for comparable one-part geopolymers. This is attributed to an almost complete reaction of the RHA and the absence of crystalline byproducts (zeolites) in the hardened geopolymer.
Als umweltschonende Alternative zu portlandzementgebundenen
Betonen werden derzeit in der Betonindustrie und in der
Baustoffforschung Betone mit alkaliaktivierten Bindemitteln,
sog. Geopolymerbetone, intensiv erforscht. Die auf industriellen
Reststoffen wie Flugasche und Hüttensand basierenden anorganischen
Bindemittel weisen bei geeigneter Zusammensetzung
einen hohen Widerstand gegenüber aggressiven Salzlösungen
und Säuren auf. Als Grundlage für den rechnerischen
Nachweis der Tragfähigkeit von brandbeanspruchten Betonbauteilen
auf Basis von alkaliaktivierten Bindemitteln werden
deshalb an der Bundesanstalt für Materialforschung und -prüfung
(BAM) die mechanischen Hochtemperatureigenschaften
von flugaschebasierten Geopolymerbetonen systematisch
untersucht.
Die bis zu 750 °C erhitzten Probekörper mit quarzitischer
und leichter Gesteinskörnung zeigen einen Festigkeitsverlust
bis ca. 300 °C, der auf entwässerungsbedingte Mikrorissbildung
zurückgeführt werden kann. Bei weiter zunehmender
Temperatur steigt aufgrund von Sinterungsprozessen ab
ca. 500 °C die Festigkeit der untersuchten Geopolymerbetone
wieder an. Diese im Vergleich zu herkömmlichem Beton günstigere
Materialeigenschaft eröffnet potenziell auch Anwendungsmöglichkeiten
in brandschutztechnisch kritischen Infrastrukturbereichen.
Die Ergebnisse der thermomechanischen
Prüfungen werden für numerische Bauteilberechnungen als
temperaturabhängige Spannungs-Dehnungs-Beziehungen aufbereitet.
Wesentlich für das Sicherheitsniveau und damit die nachhaltige Wettbewerbsfähigkeit des Technologiestandortes Deutschland ist der Brandschutz in Industrieanlagen, in Gebäuden und im Transportwesen. Der vorbeugende bauliche Brandschutz hat u. a. das Ziel, die Brand- und Rauchausbreitung im Brandfall für eine gewisse Zeit zu behindern, damit die erforderlichen Lösch- und Rettungsarbeiten durchgeführt werden können. Dies geschieht u.a. durch Anforderungen an die Feuerwiderstandsfähigkeit brandbeanspruchter Bauteile. Der Feuerwiderstand eines Bauteils ist die Fähigkeit während eines angegebenen Zeitraums in einer genormten Feuerwiderstandsprüfung bezüglich mechanischer Stabilität und/oder thermischer Isolierung nicht zu versagen. Reaktive Brandschutzbeschichtungen erhöhen für viele Bauteile sehr effektiv den Feuerwiderstand. Die Beschichtungen und die Brandprüfungen müssen jedoch an die immer komplexeren Anwendungen und/oder extremeren Anforderungen angepasst und weiterentwickelt werden. Aktuelle Forschungsschwerpunkte liegen dabei in der Entwicklung neuer Materialien (z.B. Geopolymere, keramisierende Beschichtungen, silikonbasierte Beschichtungen) für extreme Brandszenarien (extreme Temperaturen, lange Beanspruchungszeiten) und in der Realisierung komplexer Funktionalitäten (komplexe Geometrien, bewegliche Komponenten) sowie in der Entwicklung neuer Testmethoden (Feuerwiderstand als bench-scale Tests, kostengünstiges Screening, Feuerwiderstand in extremen Brandszenarien). Die Entwicklung geht dabei weg von der präskriptiven Bewertung hin zur leistungsorientierten (performance-based) Bewertung in individuellen Brandszenarien oder von komplexen Bauteilen. Im Rahmen dieser Arbeit werden Lösungsansätze für die neuen Herausforderungen an die reaktiven Brandschutzsysteme unter Extrembedingungen und deren Testmöglichkeiten vorgestellt und diskutiert. Im Mittelpunkt stehen dabei neu entwickelte bench-scale Testmethoden zum Screening von neuen Beschichtungsmaterialien sowie zur Beurteilung spezieller bzw. materialspezifischer Aspekte des Feuerwiderstands unter Extrembedingungen.
Two fly ash-based geopolymer concretes with quartz aggregates or with expanded clay (lightweight) aggregates were exposed to the ISO 834-1 standard fire curve in a small-scale fire test set-up. Acoustic emission measurements during fire exposure and subsequent cooling were employed to study spalling events and cracking during the tests. Optical microscopy and additional acoustic measurements were conducted after the testing to better understand the crack propagation in the samples. The testing revealed that neither of the concretes were susceptible to spalling, which is particularly notable for the concrete with quartz aggregates, as it is a high-strength concrete. This behavior is attributed to the relatively high permeability of the concretes and their low amount of chemically bound water. Significant crack formation was detected only around the temperature of the alpha–beta quartz transition (573 °C) and on cooling. Because of aggregate deformations at the quartz transition temperature, deterioration after heating was more significant in the geopolymer concrete with quartz aggregates. Crack formation also occurred in the concrete with expanded clay aggregates, caused by shrinkage of the geopolymer paste on cooling. Acoustic emission measurements proved to be a valuable tool to investigate processes during high temperature exposure.
The mechanical and microstructural properties of geopolymer concretes were assessed before, during and after high temperature exposure in order to better understand the engineering properties of the material. Fly ash based geopolymer concretes with either quartz aggregate or expanded clay aggregate were exposed to various temperatures up to 750 °C using a thermo-mechanical testing apparatus. Microstructural investigations were also undertaken to better understand the measured changes in the mechanical properties. It was found that dehydration of capillary water caused cracking and strength losses at temperatures ≤300 °C, an effect that was more severe in the quartz aggregate geopolymer due to its lower permeability. At higher temperatures (T ≥ 500 °C) sintering promoted strength increases which enabled both concrete types to yield significant strength advantages over conventional materials. Stress–mechanical strain curves, which form the basis of the fire design of concrete structures, are reported.
One-part geopolymers were synthesized from two different silica materials (a silica-rich residue from chlorosilane production and a commercial microsilica) and sodium aluminate at three different SiO2/Al2O3 ratios and a nominal water/solids ratio of 0.5. The degree of reaction of the silica in the cured geopolymers (i.e. the fraction of silica dissolved to form aluminosilicates and minor products) was determined using two different methods: chemical attack with HCl to dissolve the reaction products and evaluation of peak areas of 29Si MAS NMR spectra. It was found that the degree of reaction of the silica decreases with increasing the silica content of the starting mix, and that it is almost constant after 1 day of curing and almost independent from the kind of starting silica. From the results of the NMR-based method, the mean SiO2/Al2O3 ratio of the reaction products (aluminosilicates and minor products) can be estimated to be ca. 2.0, nearly independent of the starting composition of the geopolymers. The dissolution method is biased, but of sufficient precision to be useful for following changes of the degree of reaction. Major crystalline phases in the cured geopolymers are zeolite A and/or hydrosodalite. Depending on the starting composition, the relative amounts of these zeolites vary; additionally, sodalite (only for the residue from chlorosilane production with >1 wt% Cl-), faujasite, and zeolite EMT can appear in the geopolymers. The 29Si and 27Al MAS NMR results indicate mainly Si(4Al) and Al(4Si) sites, in line with the presence of zeolite A, hydrosodalite, sodalite, and geopolymeric gel of comparatively low SiO2/Al2O3 ratio.
Geopolymer-zeolite composites were synthesized using a silica-rich industrial byproduct from chlorosilane production and sodium aluminate. Pastes were cured at 80 °C and 80% RH, and subsequently dried in two different climates: at 23 °C and 50% RH, and under vacuum. 1H MAS, 23Na MAS and 29Si MAS NMR and XRD measurements were performed after the drying procedures as well as after subsequent aging. Zeolite Na-A was found beside traces of faujasite-type zeolite and zeolite EMT as major crystalline phases in the cured composites; the fraction of geopolymeric gel in the reaction products was determined to be ~18% on a molar basis. Various water species could be distinguished using 1H MAS and 1H-29Si CP MAS NMR, applying rotorsynchronized echo experiments. The largest fraction of the pore water resides in the α-cages of the zeolite Na-A and in the geopolymeric gel; in addition, water exists in the β-cages of the zeolites and adsorbed at sodium ions. The water species in α-cages and in the pores of the geopolymeric gel exhibit slightly different chemical shifts of 4.7 ppm and 4.9 ppm, respectively, in the 1H MAS NMR spectra. Changes of the water content in the geopolymer pores of differently dried samples were observed and led to slightly varied chemical shifts in the 29Si MAS NMR spectra too. Measurements after more than 500 days revealed no significant aging effects of the composites, which confirm their chemical stability.
This contribution presents the results of structural and compressive strength investigations on cured andhigh-temperature treated silica-based one-part geopolymer-zeolite composites. The specimens weresynthesized from two different silica sources, sodium aluminate and water. The phase content as well asthe compressive strength of the cured composites varied depending on the starting mix-design and thesilica feedstock. Besides geopolymeric gel, A-type zeolites and hydrosodalites were the major reactionproducts. One of the silica feedstocks yielded significantly higher compressive strength (19 MPa), whilethe other one appears to cause less variation in phase content. Strength testing indicated an improvementon heating up to
200–400 °C (28 MPa) followed by a moderate decrease up to 700 °C. Above 700 °C the sys-tems underwent new phase formation and shrinkage (volume decrease) deformations. After exposureat 1000 °C the different mixes consisted of a mix of several stuffed silica phases, almost pure hexago-nal nepheline or amorphous phase. Depending on the mix-design, the onset temperature of the hightemperature phase transformations varied.