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At least 19 records

Effective properties of a fly ash geopolymer: Synergistic application of X-ray synchrotron tomography, nanoindentation, and homogenization models

Microstructural and micromechanical investigation of a fly ash-based geopolymer using: (i) synchrotron X-ray tomography (XRT) to determine the volume fraction and tortuosity of pores that are influential in fluid transport, (ii) mercury intrusion porosimetry (MIP) to capture the volume fraction of smaller pores, (iii) scanning electron microscopy (SEM) combined with multi-label thresholding to identify and characterize the solid phases in the microstructure, and (iv) nanoindentation to determine the component phase elastic properties using statistical deconvolution, is reported in this paper. The phase volume fractions and elastic properties are used in multi-step mean field homogenization (Mori–Tanaka and double inclusion) models to determine the homogenized macroscale elastic modulus of the composite. The homogenized elastic moduli are in good agreement with the flexural elastic modulus determined on macroscale paste beams. The combined use of microstructural and micromechanical characterization tools at multiple scales provides valuable information towards the material design of fly ash geopolymers.

36 MATERIALS SCIENCE↗

Mineral assemblage transformation of a metakaolin-based waste form after geopolymer encapsulation

Current plans for nuclear waste vitrification at the Hanford Tank Waste Treatment and Immobilization Plant (WTP) lack the capacity to treat all of the low activity waste (LAW) that is not encapsulated in the vitrified product. Fluidized Bed Steam Reforming (FBSR) is one of the supplemental technologies under consideration to fill this gap. The FBSR process results in a granular product mainly composed of feldspathoid mineral phases that encapsulate the LAW and other contaminants of concern (COCs). In order to better understand the characteristics of the FBSR product, characterization testing has been performed on the granular product as well as the granular product encapsulated in a monolithic geopolymer binder. The non-radioactive simulated tank waste samples created for use in this study are the result of a 2008 Department of Energy sponsored Engineering Scale Technology Demonstration (ESTD) in 2008. These samples were created from waste simulant that was chemically shimmed to resemble actual tank waste, and rhenium has been used as a substitute for technetium. Another set of samples was created by the Savannah River Site Bench-Scale Reformer (BSR) using a chemical shim of Savannah River Site Tank 50 waste in order to simulate a blend of 68 Hanford tank wastes. This paper presents results from coal and moisture removal tests along with XRD, SEM, and BET analyses showing that the major mineral components are predominantly sodium aluminosilicate minerals and that the mineral product is highly porous. Results also show that the materials pass the short-term leach tests: the Toxicity Characteristic Leaching Procedure (TCLP) and Product Consistency Test (PCT).

Feldspathoid Minerals↗

Geopolymer resin materials, geopolymer materials, and materials produced thereby

A product formed from a first material including a geopolymer resin material, a geopolymer resin, or a combination thereof by contacting the first material with a fluid and removing at least some of the fluid to yield a product. The first material may be formed by heating and/or aging an initial geopolymer resin material to yield the first material before contacting the first material with the fluid. In some cases, contacting the first material with the fluid breaks up or disintegrates the first material (e.g., in response to contact with the fluid and in the absence of external mechanical stress), thereby forming particles having an external dimension in a range between 1 nm and 2 cm.

36 MATERIALS SCIENCE↗

Geopolymer resin materials, geopolymer materials, and materials produced thereby

A product formed from a first material including a geopolymer resin material, a geopolymer material, or a combination thereof by contacting the first material with a fluid and removing at least some of the fluid to yield a product. The first material may be formed by heating and/or aging an initial geopolymer resin material to yield the first material before contacting the first material with the fluid. In some cases, contacting the first material with the fluid breaks up or disintegrates the first material (e.g., in response to contact with the fluid and in the absence of external mechanical stress), thereby forming particles having an external dimension in a range between 1 nm and 2 cm.

36 MATERIALS SCIENCE↗

Magnetic fly-ash geopolymer for heavy metal removal in aqueous solutions

Novel magnetic geopolymers were manufactured by synthesizing magnetic Fe 3 O 4 particles on the surface of prepared geopolymer (Method 1) or by incorporating pre-synthesized magnetic Fe 3 O 4 particles into the geopolymer during the manufacture of the geopolymer (Method 2). This study evaluated the effect of the incorporated magnetic Fe 3 O 4 on the geopolymer magnetic, physical, and adsorption properties and its separation in aqueous solutions. Based on several preliminary measurements on the synthesized magnetic geopolymers, Method 2 was found to be a better method for producing magnetic geopolymer. Magnetic geopolymer synthesized by Method 2 exhibited ferromagnetic properties comparable to that of magnetic Fe 3 O 4 , with a saturation magnetization of 8 emu·g −1 and an intrinsic coercivity of 265 Oe. The magnetic geopolymer was efficiently separated from an aqueous solution within 2 min using a 0.48-T magnetic field. In addition, the magnetic geopolymer has a maximum copper adsorption capacity of 111.1 mg·g −1 , which was similar to the non-magnetic reference geopolymer indicating that the addition of magnetic Fe 3 O 4 did not compromise the geopolymer adsorption capacity. The magnetic geopolymer is a promising material with good adsorption and separation properties that can be used for heavy metals removal and recovery in wastewater and metals separation in industrial processes.

fly ash↗

Study on Application of Geopolymer to the Retrieval of Fuel Debris in Fukushima Dai-ichi NPP

In order to retrieve fuel debris in Fukushima Dai-ichi NPP, many retrieval methods are proposed. Geopolymer is the candidate material applied for an alternative retrieval method. In this concept, Geopolymer can be used to stabilize fuel debris and suppress the diffusion of radioactive materials. Objective: Evaluation of geopolymer applied for retrieving fuel debris. Slump Flow Test: Slump flow values decreased as the test temperature increased. In air condition, water molecules evaporated from geopolymer and the viscosity of geopolymer increased. In water condition, the same trends as in air condition were observed. Slump flow values of geopolymer also depended on the elapsed time after mixing. By adding water, the slump flow values of geopolymer became higher (Even at 80 deg. C). It is possible to adjust the solidification time (Setting time) of geopolymer. Solidification Process of Geopolymer: After the first layer solidified, the second layer was injected. At 300 deg. C, porous structure was observed in the first layer, while the second layer structure was intact. In the actual application, multilayered geopolymer may be used to stabilize fuel debris. Conclusion: Fluidity of geopolymer decreased with raising temperature. Setting time can be adjusted by adding water. Geopolymer may be applied by injecting multiple times on high temperature materials above 100 deg. C.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Comparison on the properties of ITZs in fly ash-based geopolymer and Portland cement concretes with equivalent flowability

Highlights: • Modelled ITZs can effectively avoid the effects caused by different factors and test locations of ITZ. • ITZ properties of PC and geopolymer concretes are compared based on equivalent flowability of binders. • Geopolymer ITZ exhibits stronger bonding than that of PC, and higher mechanical properties than geopolymer paste. • Strong ITZs in geopolymer concrete are attributed to the layer of gel-rich paste with dense microstructures. • Elastic modulus and hardness properties of ITZs in PC concrete are increased due to the CH crystals. This paper aims to compare the properties of interfacial transition zones (ITZs) in Portland cement (PC) concrete and geopolymer concrete. Portland cement and geopolymer pastes were designed with the equivalent flowability to provide similar mix and casting condition of ITZs. Two types of modelled ITZs were prepared to facilitate the nanoindentations across ITZs, microstructural characterization, and comparison on the properties of ITZs with less influential factors. The results showed that the interfacial bonding of ITZs between geopolymer matrix and aggregate is relatively stronger than the counterpart in the PC concrete. There is a high amount of crystalline hydration products in the ITZs of PC concrete, but a layer gel-rich paste with denser microstructures in the ITZs of geopolymer concrete. Additionally, the interface morphology and nanoindentation analysis indicate that the property of ITZs in the modelled geopolymer concrete is not poorer than that of the corresponding geopolymer paste.

36 MATERIALS SCIENCE↗

Immobilization of Radioactive Wastes Using Geopolymers - 19483

This work explores an encapsulation and immobilization technology for spent radioactive ion exchange (IX) resins using geopolymer materials as a matrix. Geopolymer-IX resin composites with different IX resin loadings were prepared by mixing an aluminosilicate material (metakaolin), sodium hydroxide and inactive IX resin (Amberlite IRN 150) and curing the mixture at room temperature with or without γradiation applied using an external radiation source. The metakaolin and sodium hydroxide reacted to form a geopolymer framework encapsulating the IX resin beads. The IX resin loading capacity and the encapsulation efficiency of the geopolymer material were investigated by examining the morphology and distribution of resins within the geopolymer framework using optical microscopy, and by measuring the compressive strengths of the geopolymer-IX resin composites. These properties of the geopolymer-IX resin composites were compared with those of ordinary Portland cement (OPC)-IX resin composites. The geopolymer matrix allowed for a higher IX resin loading capacity than OPC. The geopolymer-IX resin composite was stable under γ-radiation for 28 d. In leaching tests performed with encapsulated Sr-loaded IX resins, the ability of the geopolymer to prevent leaching of Sr{sup 2+} into solution was greatly superior to that of OPC. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Utilisation of steel furnace slag coarse aggregate in a low calcium fly ash geopolymer concrete

This paper evaluates the performance of steel furnace slag (SFS) coarse aggregate in blended slag and low calcium fly ash geopolymer concrete (GPC). The geopolymer binder is composed of 90% of low calcium fly ash and 10% of ground granulated blast furnace slag (GGBFS). Mechanical and physical properties, shrinkage, and detailed microstructure analysis were carried out. The results showed that geopolymer concrete with SFS aggregate offered higher compressive strength, surface resistivity and pulse velocity than that of GPC with traditional aggregate. The shrinkage results showed no expansion or swelling due to delayed calcium oxide (CaO) hydration after 320 days. No traditional porous interfacial transition zone (ITZ) was detected using scanning electron microscopy, indicating a better bond between SFS aggregate and geopolymer matrix. Energy dispersive spectroscopy results further revealed calcium (Ca) diffusion at the vicinity of ITZ. Raman spectroscopy results showed no new crystalline phase formed due to Ca diffusion. X-ray fluorescence result showed Mg diffusion from SFS aggregate towards geopolymer matrix. The incorporation of Ca and Mg into the geopolymer structure and better bond between SFS aggregate and geopolymer matrix are the most likely reasons for the higher compressive strength observed in GPC with SFS aggregate.

36 MATERIALS SCIENCE↗

Chemo–mechanical properties of carbon fiber reinforced geopolymer interphase

Geopolymers, as a potentially environmentally friendly alternative to Portland cement, are increasingly attracting attention in the construction industry. Various methods have been applied for customizing the properties of geopolymers and improving their commercial viability. One of the promising methods for refining the properties of geopolymers such as their toughness is the use of short fibers. The effectiveness of a high-strength short fiber in the geopolymer matrix is largely dependent on the interfacial bonding between the fiber and its surrounding matrix. While the importance of this interfacial chemistry is highlighted in the literature, the characteristics of this bonding structure have not been fully understood. In this paper, we aim to investigate the bonding mechanism between the carbon fiber and metakaolin-based geopolymer matrix. For the first time, the existence and nature of the chemical bonding at the interfacial region (interphase) between carbon fiber and geopolymer matrix has been revealed. X-ray pair distribution function computed tomography (PDF-CT), field emission-scanning electron microscopy imaging, and nanoindentation techniques are employed to discern the chemo-mechanical properties of the interphase. PDF-CT results show the emergence of a new atom-atom correlation at the interfacial region (around 1.82 angstrom). This correlation is a characteristic of interfacial bonding between the fiber and its surrounding matrix, where the existence of chemical linkages (potentially Al-V-O-C) between fibers and the matrix contributes to the adhesion between the two constituents making up the composite. Due to such chemical bonding, the nanomechanical properties of the interfacial region fall between that of the carbon fiber and geopolymer. The combination of advanced techniques is proved useful for enhancing our understanding of the interfacial chemistry between fibers and the binding matrix. This level of knowledge facilitates the engineering of composite systems through the manipulation of their nanostructure.

36 MATERIALS SCIENCE↗

Transformations of Na, Al, Si and Fe species in red mud during synthesis of one-part geopolymers

Reaction mechanism of one-part geopolymer formation using red mud (RM) was explored in this study. Leaching test, X-ray photoelectron spectroscopy (XPS), Mössbauer spectroscopy and nitrogen isothermal adsorption (NIA) were conducted to study transformations of Na, Al, Si, Fe species, binding energies of Al−O and Si−O, and pore structure, respectively. The alkali-thermal-activated RM could dissolve in water to release large amounts of soluble Na, Al and Si species for geopolymerization. But more dissolved Si is needed from added silica fume (SF) to form stable geopolymer gels. The binding energies of Al−O and Si−O bonds in the geopolymer increased with the polymerization of reactive SiO{sub 2} and Al{sub 2}O{sub 3}. The coordinated Fe{sup 3+} in RM played a role like Al{sup 3+} by replacing it in the aluminosilicates structure, and exerted no obvious impact on geopolymerization. The dissolved SF took part in the geopolymerization to form dense geopolymer matrices in long-term curing. - Highlights: • Large amounts of Na, Al and Si dissolved from alkali-thermal-activated RM in water. • Low Si/Al geopolymers will dissolve and release soluble Al in long-term curing. • Dissolved Si from SF participates in the polymerization of soluble Na, Al and Si. • The binding energies of Al−O and Si−O will increase after geopolymerization. • The coordinated Fe{sup 3+} replaces Al{sup 3+} in aluminosilicate structure of geopolymer.

36 MATERIALS SCIENCE↗

Understanding geopolymer binder-aggregate interfacial characteristics at molecular level

The interfacial characteristics of geopolymer binder to aggregate composites are poorly understood, especially at molecular level. Herein, molecular models are developed to study, for the first time, the geopolymer-aggregate interface. Chemically, various forms of interfacial bonding are characterized, including Al-O-Si bonding through condensation reactions, NaO and H-bonding. An atomic-level interfacial transition zone (ITZ) is identified, attributed to the concentration of –OH groups. Increasing the Si/Al ratio of geopolymer is found to decrease the ITZ density, but have limited effect on the ITZ width. A heterogeneous diffusion characteristic occurs in geopolymer, due to the weak interfacial interaction. Mechanically, lowering the Si/Al ratio promotes the interfacial strength due to the stronger interfacial interaction and higher cross-linking degree in geopolymer. Under loading the interfacial fracture undergoes three stages: crack propagation, chain bridging (including aluminosilicate and ionic bridging) and breakage. The above atomic-level findings may facilitate a better design of geopolymer concrete in engineering.

36 MATERIALS SCIENCE↗

Studies on Workability of Geopolymer Solidification - 18171

In Japan, intermediate-level radioactive waste, such as spent resin, is solidified and set in sealed containers without venting. To reduce the amount of hydrogen generated due to water radiolysis in stored intermediate-level waste, geopolymer solidification has been studied. Geopolymer solidification is an excellent method for conditioning intermediate-level waste from the viewpoint of its high thermal stability and low processing cost. However, it has a problem that the apparent viscosity increases drastically a few minutes after the onset of setting. This may cause some trouble in the process of pouring the geopolymer into drums and mixing it with waste. In this study, in order to control the workability of a geopolymer mixture, we investigated the effects of the compounding ratio and the kinds of chemical agents used. We confirmed that the geopolymer reaction was slowed down by reducing the amount of calcium and adding boron. The uniaxial compressive strength of the geopolymer was 3-80 MPa. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Landfilled coal ash for carbon dioxide capture and its potential as a geopolymer binder for hazardous waste remediation

In this report, the legacy of global fossil fuel usage is not just the increase in global warming due to CO 2 production, but also the billions of tons of toxic coal ash disposed in landfills. This investigation evaluates the merits of using high-calcium landfilled coal fly ash of different disposal durations and granulated blast furnace (GBF) slag as primary raw materials for production of a new class of geopolymer binder. Processing of landfilled coal fly ash, GBF slag and supplementary raw materials into a geopolymer binder was accomplished by a simple, scalable milling process in the absence of heating under a carbon dioxide environment. The resultant geopolymer cement binders were tested for carbon dioxide uptake, compressive strength, and heavy metal stabilization. The geopolymer binder demonstrated a desired balance of carbon dioxide uptake, strength and safety. These results also indicate that the performance of the geopolymer binder depends on the landfill disposal age of the coal fly ash.

29 ENERGY PLANNING, POLICY, AND ECONOMY↗

Early age volume changes in metakaolin geopolymers: Insights from molecular simulations and experiments

The early age volume changes occurring during the geopolymerisation reaction are not sufficiently understood yet, due to shortage of experimental data and theoretical models. This work presents new results on chemical and autogenous deformation of sodium-activated geopolymers from metakaolin, focussing on the first 72 h of reaction. The results show that the geopolymers undergo early-age chemical expansion, not shrinkage. A model is proposed to explain the experimental result, leveraging recent advances from molecular simulations. The model predicts how the extent of chemical expansion is controlled by confined water in the molecular structure of the geopolymer. However, despite this underlying chemical expansion, geopolymer samples undergo autogenous shrinkage at the macroscale, which excludes self-desiccation as the origin of autogenous deformation. A better insight is gained by monitoring the kinetics of geopolymerisation using isothermal and differential calorimetry. Two kinetic regimes are identified, with apparent activation energies of approximately 90 kJ/mol and 70 kJ/mol. This suggests that two microscopic mechanisms concur to determine the early-age volume changes of geopolymer pastes.

36 MATERIALS SCIENCE↗

Characterization of geopolymer fly-ash based foams obtained with the addition of Al powder or H{sub 2}O{sub 2} as foaming agents

Recent innovations in geopolymer technology have led to the development of various different types of geopolymeric products, including highly porous geopolymer-based foams, which are formed by the addition of foaming agents to a geopolymer fly-ash based matrix. These agents decompose, or react with the liquid matrix or oxygen in the matrix, resulting in the release of gases which form pores prior to the hardening of the gel. The hardened structure has good mechanical and thermal properties, and can therefore be used for applications in acoustic panels and in lightweight pre-fabricated components for thermal insulation purposes. This study presents the results of the pore-forming process in the case when two different foaming agents, i.e. aluminium powder amounting to 0.07, 0.13 and 0.20 mass. % and H{sub 2}O{sub 2} amounting to 0.5, 1.0, 1.5 and 2.0 mass. %, were added to a fly-ash geopolymer matrix. The physical, mechanical, and microstructural properties of the thus obtained foams, and the effects of the type and amount of the added foaming agent, are presented and discussed. Highly porous structures were obtained in the case of both of the investigated foaming agents, with overall porosities up to 59% when aluminium powder was added, and of up 48% when H{sub 2}O{sub 2} was added. In the latter case, when 2% of the H{sub 2}O{sub 2} foaming agent was added, finer pores (with diameters up to 500 μm) occurred in the structure, whereas somewhat larger pores (some had diameters greater than 1 mm) occurred when the same amount of aluminium powder was added. The mechanical properties of the investigated foams depended on their porosity. In the case of highly porous structures a compressive strength of 3.3 MPa was nevertheless achieved for the samples containing 0.2% of aluminium powder, and 3.7 MPa for those containing 2.0% of H{sub 2}O{sub 2}. - Highlights: • Preparation of geopolymer foams based on fly ash with the addition of Al powder or H{sub 2}O{sub 2} as foaming agents • Determination of density, porosity and mechanical properties of such foams • Characterization of foaming process by means of X-ray micro-tomography (μcT)

36 MATERIALS SCIENCE↗

Properties of Geopolymer Composites Reinforced with Basalt Chopped Strand Mat or Woven Fabric

Geopolymers or polysialates are inorganic polymeric, ceramic‐like materials composed of alumina, silica, and alkali metal oxides that can be made without any thermal treatment. Additions of reinforcing phases vastly improve the mechanical properties and high‐temperature stability of the geopolymer. The processing and mechanical properties of both chopped strand mat as well as 2‐D woven fabric‐reinforced potassium geopolymer composites have been evaluated. Hand lay‐up and hydraulic press processing methods were used to produce composite panels. The room‐temperature tensile and flexural strength of chopped strand mat composites was 21.0 ± 3.1 and 31.7 ± 4.4 MP a, respectively, while those of basalt weave‐reinforced geopolymer composites reached 40.0 ± 5.9 and 45.2 ± 9.3 MP a, respectively. Composite microstructures were examined using optical microscopy as well as scanning electron microscopy ( SEM ). Mass, volume, and porosity fractions were also determined. The effect of high‐temperature treatments at 25°C, 300°C, 600°C, and 800°C were analyzed. Finally, Weibull statistical analysis was performed, which showed an increase in reliability when a reinforcement phase was added to K‐geopolymer.

Ribero, Daniel↗