Search results for: aluminate

Authors: Tao Liu, Qingliang Yu, H. J. H. Brouwers

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Among the reaction products in the alkali-activated ground granulated blast furnace slag (AAS), the layered double hydroxides (LDHs) have a remarkable capacity of chloride and heavy metal ions absorption. The promotion of LDH phases in the AAS matrix can increase chloride resistance. The objective of this study is that use the different dosages of sodium aluminate to activate slag, consequently promoting the formation of in-situ LDH. The hydration kinetics of the sodium aluminate activated slag (SAAS) was tested by the isothermal calorimetry. Meanwhile, the reaction products were determined by X-ray diffraction (XRD), thermogravimetric analysis (TGA), and Fourier-transform infrared spectroscopy (FTIR). The sodium hydroxide-activated slag is selected as the reference. The results of XRD, TGA, and FTIR showed that the formation of LDH in SAAS was increased by the aluminate dosages.

Keywords: ground granulated blast furnace slag, sodium aluminate activated slag, in-situ LDH formation, chloride absorption

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Authors: Ji Hoi Heo, Jun Seong Park, Hyo Kim

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Geopolymer is an inorganic material synthesized by alkali activation of source materials rich in soluble SiO₂ and Al₂O₃. Many researches have studied the effect of aluminum species on the synthesis of geopolymer. However, it is still unclear about the influence of Al additives on the properties of geopolymer. The current study identified the role of the Al additive on the thermal performance of fly ash based geopolymer and observing the microstructure development of the composite. NaOH pellets were dissolved in water for 14 M (14 moles/L) sodium hydroxide solution which was used as an alkali activator. The weight ratio of alkali activator to fly ash was 0.40. Sodium aluminate powder was employed as an Al additive and added in amounts of 0.5 wt.% to 2 wt.% by the weight of fly ash. The mixture of alkali activator and fly ash was cured in a 75°C dry oven for 24 hours. Then, the hardened geopolymer samples were exposed to 300°C, 600°C and 900°C for 2 hours, respectively. The initial compressive strength after oven curing increased with increasing sodium aluminate content. It was also observed in SEM results that more amounts of geopolymer composite were synthesized as sodium aluminate was added. The compressive strength increased with increasing heating temperature from 300°C to 600°C regardless of sodium aluminate addition. It was consistent with the ATR-FTIR results that the peak position related to asymmetric stretching vibrations of Si-O-T (T: Si or Al) shifted to higher wavenumber as the heating temperature increased, indicating the further geopolymer reaction. In addition, geopolymer sample with higher content of sodium aluminate showed better compressive strength. It was also reflected on the IR results by more shift of the peak position assigned to Si-O-T toward the higher wavenumber. However, the compressive strength decreased after being exposed to 900°C in all samples. The degree of reduction in compressive strength was decreased with increasing sodium aluminate content. The deterioration in compressive strength was most severe in the geopolymer sample without sodium aluminate additive, while the samples with sodium aluminate addition showed better thermal durability at 900°C. This is related to the phase transformation with the occurrence of nepheline phase at 900°C, which was most predominant in the sample without sodium aluminate. In this work, it was concluded that sodium aluminate could be a good additive in the geopolymer synthesis by showing the improved compressive strength at elevated temperatures.

Keywords: compressive strength, fly ash based geopolymer, microstructure development, Na-aluminate

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Authors: Linlin Wang, Guangdong Bian, Jifeng Shen, Jingzhu Zeng

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Zinc-aluminum alloys have been applied as alternatives to bronze, aluminum alloys, and cast iron due to their distinguishing features such as high as-cast strength, excellent bearing properties, as well as low energy requirements for melting. In this study, oxide coatings were produced on ZA27 zinc-aluminum alloy by a plasma electrolytic oxidation (PEO) method. Three coatings were deposited by using three various electrolytes, i.e. silicate, aluminate and aluminate/borate composite solutions. The current density is set at 0.1A/cm2, deposition time is 40 mins for all the deposition processes. The surface morphology and phase structure of the three coatings were characterized by scanning electron microscopy （SEM） and X-ray diffraction (XRD). Pin-on-disc sliding wear tests were conducted to test the tribological properties of coatings. The results indicated that the coating produced using the aluminate/borate composite electrolyte had the highest deposition rate and best wear resistance among the three coatings.

Keywords: oxide coating, PEO, tribological properties, ZA27

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Authors: Konstantinos Sotiriadis, Radosław Mróz

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In the present work the internal sulfate attack on pastes made from pure clinker phases was studied. Two binders were produced: (a) a binder with 2% C3A and 18% C4AF content; (b) a binder with 10% C3A and C4AF content each. Gypsum was used as the sulfate bearing compound, while calcium carbonate added to differentiate the binders produced. The phases formed were identified by XRD analysis. The results showed that ettringite was the deterioration phase detected in the case of the low C3A content binder. Carbonation occurred in the specimen without calcium carbonate addition, while portlandite was observed in the one containing calcium carbonate. In the case of the high C3A content binder, traces of thaumasite were detected when calcium carbonate was not incorporated in the binder. A solid solution of thaumasite and ettringite was found when calcium carbonate was added. The amount of C3A had not fully reacted with sulfates, since its corresponding peaks were detected.

Keywords: tricalcium aluminate, calcium aluminate ferrite, sulfate attack, calcium carbonate, low temperature

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Authors: Ghayah Alsaleem

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This research project focussed on specific compounds, whereas a literature review was completed on the broader subject of long-lasting phosphorescence. For the review and subsequent laboratory work, long lasting phosphorescence compounds were defined as materials that have an afterglow decay time greater than a few minutes. The decay time is defined as the time between the end of excitation and the moment the light intensity drops below 0.32mcd/m2. This definition is widely used in industry and in most research studies. The experimental work focused on known long-lasting phosphorescence compounds – strontium aluminate (SrAl2O4: Eu2+, Dy3+). At first, preparation was similar to literary methods. Temperature, dopant levels and mixing methods were then varied in order to expose their effects on long-lasting phosphorescence. The effect of temperature was investigated for SrAl2O4: Eu2+, Dy3+, and resulted in the discovery that 1350°C was the only temperature that the compound could be heated to in the Differential scanning calorimetry (DSC) in order to achieve any phosphorescence. However, no temperatures above 1350°C were investigated. The variation of mixing method and co-dopant level in the strontium aluminate compounds resulted in the finding that the dry mixing method using a Turbula mixer resulted in the longest afterglow. It was also found that an increase of europium inclusion, from 1mol% to 2mol% in these compounds, increased the brightest of the phosphorescence. As this increased batch was mixed using sonication, the phosphorescent time was actually reduced which produced green long-lasting phosphorescence for up to 20 minutes following 30 minutes excitation and 50 minutes when the europium content was doubled and mixed using sonication.

Keywords: long lasting, phosphorescence, excitation, europium

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Authors: Qian Li, Zhaoping Zhong

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Sewage sludge, a typical solid waste, has inevitably been produced in enormous quantities in China. Still worse, the amount of sewage sludge produced has been increasing due to rapid economic development and urbanization. Compared to the conventional method to treat sewage sludge, pyrolysis has been considered an economic and ecological technology because it can significantly reduce the sludge volume, completely kill pathogens, and produce valuable solid, gas, and liquid products. However, the large-scale utilization of sludge biochar has been limited due to the considerable risk posed by heavy metals in the sludge. Heavy metals enriched in pyrolytic biochar could be divided into exchangeable, reducible, oxidizable, and residual forms. The residual form of heavy metals is the most stable and cannot be used by organisms. Kaolin and zeolite are environmentally friendly inorganic minerals with a high surface area and heat resistance characteristics. So, they exhibit the enormous potential to immobilize heavy metals. In order to reduce the risk of leaching heavy metals in the pyrolysis biochar, this study pyrolyzed sewage sludge mixed with kaolin/zeolite in a small rotary kiln. The influences of additives and pyrolysis temperature on the leaching concentration and morphological transformation of heavy metals in pyrolysis biochar were investigated. The potential mechanism of stabilizing heavy metals in the co-pyrolysis of sludge blended with kaolin/zeolite was explained by scanning electron microscopy, X-ray diffraction, and specific surface area and porosity analysis. The European Community Bureau of Reference sequential extraction procedure has been applied to analyze the forms of heavy metals in sludge and pyrolysis biochar. All the concentrations of heavy metals were examined by flame atomic absorption spectrophotometry. Compared with the proportions of heavy metals associated with the F4 fraction in pyrolytic carbon prepared without additional agents, those in carbon obtained by co-pyrolysis of sludge and kaolin/zeolite increased. Increasing the additive dosage could improve the proportions of the stable fraction of various heavy metals in biochar. Kaolin exhibited a better effect on stabilizing heavy metals than zeolite. Aluminosilicate additives with excellent adsorption performance could capture more released heavy metals during sludge pyrolysis. Then heavy metal ions would react with the oxygen ions of additives to form silicate and aluminate, causing the conversion of heavy metals from unstable fractions (sulfate, chloride, etc.) to stable fractions (silicate, aluminate, etc.). This study reveals that the efficiency of stabilizing heavy metals depends on the formation of stable mineral compounds containing heavy metals in pyrolysis biochar.

Keywords: co-pyrolysis, heavy metals, immobilization mechanism, sewage sludge

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Authors: Zhen Qin, Yufei Peng, Jianbei Li, Jidong Long

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In order to study the activity of the coated aluminate barium-tungsten cathodes during activation, aging, poisoning and long-term use. Through a set of hot-cathode micro-area emission uniformity study device, we tested the micro-area emission performance of the cathode under different conditions. The change of activity of cathode micro-area was obtained. The influence of micro-area activity on the performance of the cathode was explained by the ageing model of barium-tungsten cathode. This helps to improve the design and process of the cathode and can point the way in finding the factors that affect life in the cathode operation.

Keywords: barium-tungsten cathode, ageing model, micro-area emission, emission uniformity

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Authors: Osama Madkhali

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GdAl₃(BO₃)₄ phosphors, incorporating Dy³+ and Dy³+/Eu³+ activators, were successfully synthesized via the gel combustion method. Powder X-ray diffraction (XRD) was utilized to ascertain phase purity and assess the impact of dopant concentration on the crystallographic structure. Photoluminescence (PL) measurements revealed that luminescence properties' intensity and lifetime varied with Dy³+ and Eu³+ ion concentrations. The relationship between luminescence intensity and doping concentration was explored in the context of the energy transfer process between Eu³+ and Dy³+ ions. An increase in Eu³+ co-doping concentrations resulted in a decrease in luminescence lifetime. Energy transfer efficiency was significantly enhanced from 26% to 84% with Eu³+ co-doping, as evidenced by decay curve analysis. These findings position GdAl₃(BO₃)4: Dy³+, Eu³+ phosphors as promising candidates for LED applications in solid-state lighting and displays.

Keywords: GdAl₃(BO₃)₄ phosphors, Dy³+/Eu³+ co-doping, photoluminescence (PL) measurements, luminescence properties, LED applications, solid-state lighting

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Authors: Onkar Nath Verma, Nitish Kumar Singh, Raghvendra, Pravin Kumar, Prabhakar Singh

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The perovskite type electrolyte material LaAlO3 was prepared by solution based auto-combustion method using Al (NO3)3.6H2O, La2O3 with dilute nitrate acid (HNO3) as precursors and citric acid (C6H8O7.H2O) as a fuel. The synthesis protocol gave an easy processing of the LaAlO3 nano-particles. The XRD measurement revealed that the material has single phase with space group R-3c (rhombohedral). Thermal behavior was measured by simultaneous differential thermal analysis and thermo gravimetric analysis (DTA-TGA). The compact pellet density was determined. Also, the surface morphology was studied using scanning electron microscopy (SEM). The conductivity of LaAlO3 was measured employing LCR meter and found to increase with increasing temperature. This increase in conductivity may be attributed to increased mobility of oxide ion.

Keywords: perovskite, LaAlO3, XRD, SEM, DTA-TGA, SOFC

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Authors: R. Benakcha, M. Omari

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Powders of La1-xMgxAlO3 (0 ≤ x ≤ 5) oxides, with large surface areas were synthesized by sol-gel process, utilizing citric acid. Heating of a mixed solution of CA, EtOH, and nitrates of lanthanum, aluminium and magnesium at 70°C gave transparent gel without any precipitation. The formation of pure perovskite La1-xMgxAlO3, occurred when the precursor was heat-treated at 800°C for 6 h. No X-ray diffraction evidence for the presence of crystalline impurities was obtained. The La1-xMgxAlO3 powders prepared by the sol-gel method have a considerably large surface area in the range of 12.9–20 m^2.g^-1 when compared with 0.3 m^2.g^-1 for the conventional solid-state reaction of LaAlO3. The structural characteristics were examined by means of conventional techniques namely X-ray diffraction, infrared spectroscopy, thermogravimetry and differential thermal (TG-DTA) and specific surface SBET. Pore diameters and crystallite sizes are in the 8.8-11.28 nm and 25.4-30.5 nm ranges, respectively. The sol-gel method is a simple technique that has several advantages. In addition to that of not requiring high temperatures, it has the potential to synthesize many kinds of mixed oxides and obtain other materials homogeneous and large purities. It also allows formatting a variety of materials: very fine powders, fibers and films.

Keywords: aluminate, lanthan, perovskite, sol-gel

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Authors: Fadi Althoey, Yaghoob Farnam

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Sodium chloride (NaCl) can interact with the tricalcium aluminate (C3A) and its hydrates in concrete matrix. This interaction can result in formation of a harmful chemical phase as the temperature changes. It is thought that this chemical phase is embroiled in the premature concrete deterioration in the cold regions. This work examines the potential formation of the harmful chemical phase in various pastes prepared by using different types of ordinary portland cement (OPC) and supplementary cementitious materials (SCMs). The quantification of the chemical phase was done by using a low temperature differential scanning calorimetry. The results showed that the chemical phase formation can be reduced by using Type V cement (low content of C3A). The use of SCMs showed different behaviors on the formation of the chemical phase. Slag and Class F fly ash can reduce the chemical phase by the dilution of cement whereas silica fume can reduce the amount of the chemical phase by dilution and pozzolanic activates. Interestingly, the use of Class C fly ash has a negative effect on concrete exposed to NaCl through increasing the formation of the chemical phase.

Keywords: concrete, damage, chemcial phase, NaCl, SCMs

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Authors: Joanne M. Emmens

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This paper makes use of the case notes of a single psychoanalytically informed psychotherapy of a now 72-year-old man over a four-year period to explore the potential of qualitative data to be incorporated into a research methodology that can contribute theory and knowledge to the wider professional community involved in mental health care. The clinical material arising out of any psychoanalysis provides a potentially rich source of clinical data that could contribute valuably to our historical understanding of both individual and societal traumata. As psychoanalysis is primarily an investigation, it is argued that clinical case material is a rich source of qualitative data which has relevance for sociological and historical understandings and that it can potentially aluminate important ‘gaps’ and collective blind spots that manifest unconsciously and are a contributing factor in the transmission of trauma, silently across generations. By attending to this case material the hope is to illustrate the value of using a psychoanalytic centred methodology. It is argued that the study of individual defences and the manner in which they come into consciousness, allows an insight into group defences and the unconscious forces that contribute to the silencing or un-noticing of important sources (or originators) of mental suffering.

Keywords: dream furniture (Bion) and psychotic functioning, reverie, screen memories, selected fact

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Authors: Patel Darshan Shaileshkumar, M. G. Vanza

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Black cotton soil is problematic soil for any construction work. Black cotton soil contains montmorillonite in its structure. Due to this mineral, black cotton soil will attain maximum swelling and shrinkage. Due to these volume changes, it is necessary to stabilize black cotton soil before the construction of the road. For soil stabilization use of pozzolanic waste is found to be a good solution by some researchers. The palm kernel shell ash (PKSA) is a pozzolanic material that can be used for soil stabilization. Basically, PKSA is a waste material, and it is available at a cheap cost. Palm kernel shell is a waste material generated in palm oil mills. Then palm kernel shell is used in industries instead of coal for power generation. After the burning of a palm kernel shell, ash is formed; the ash is called palm kernel shell ash (PKSA). The PKSA contains a free lime content that will react chemically with the silicate and aluminate of black cotton soil and forms a C-S-H and C-A-H gel which will bines soil particles together and reduce the plasticity of the soil. In this study, the PKSA is added to the soil. It was found that with the addition of PKSA content in the soil, the liquid limit of the soil is decreased, the plastic limit of the soil is increased, and the plasticity of the soil is decreased. The group index value of the soil is evaluated, and it was found that with the addition of PKSA GI value of the soil is decreased, which indicates the strength of the soil is improved.

Keywords: palm kernel shell ash, black cotton soil, liquid limit, group index, plastic limit, plasticity index

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Authors: Rym Sassi, Franck Fayon, Mohend Chaouche, Emmanuel Veron, Valerie Montouillout

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The chemical phenomena occurring during cement hydration are complex and interdependent, and even after almost two centuries of studies, they are still difficult to solve for complex mixtures combining different hydraulic binders. Powder-XRD has been widely used for characterizing the crystalline phases in both anhydrous and hydrated cement, but only limited information is obtained in the case of strongly disordered and amorphous phases. In contrast, local spectroscopies like solid-state NMR can provide a quantitative description of noncrystalline phases. In this work, the structural modifications occurring during hydration of a fast-setting ternary binder based on white Portland cement, white calcium aluminate cement, and calcium sulfate were investigated using advanced solid-state NMR methods. We particularly focused on the early stage of the hydration up to 28 days, working with samples whose hydration was controlled and stopped. ²⁷Al MQ-MAS as well as {¹H}-²⁷Al and {¹H}-²⁹Si Cross- Polarization MAS NMR techniques were combined to distinguish all of the aluminum and silicon species formed during the hydration. The NMR quantification of the different phases was conducted in parallel with the XRD analyses. The consumption of initial products, as well as the precipitation of hydraulic phases (ettringite, monosulfate, strätlingite, CSH, and CASH), were unambiguously quantified. Finally, the drawing of the consumption and formation of phases was correlated with mechanical strength measurements.

Keywords: cement, hydration, hydrates structure, mechanical strength, NMR

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Authors: Menglim Hoy, Suksun Horpibulsuk, Arul Arulrajah

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The results of laboratory investigation of recycled asphalt pavement (RAP) – fly ash (FA) based geopolymer as a base material is presented in this paper. An alkaline activator, the mixture of NaOH and Na₂SiO₃, is used to synthesis RAP-FA based geopolymer. RAP-FA with water (RAP-FA blend) prepared as a control material. The strength develops and the strength against wet-dry was determined by the unconfined compression strength (UCS) test, then the microstructural properties were examined by scanning electron microscopy (SEM) and X-ray Diffraction (XRD) analysis. The toxicity characteristic leaching procedure (TCLP) test is conducted to measure its leachability of heavy metal. The results show both the RAP-FA blend and geopolymer can be used as a base course as its UCS values meet the minimum strength requirement specified by the Department of Highway, Thailand. The durability test results show the UCS of these materials increases with increasing the number of wet-dry cycles, reaching its peak at six wet-dry cycles. The XRD and SEM analyses indicate strength development of the RAP-FA blend occurs due to chemical reaction between a high Calcium in RAP with a high Silica and Alumina in FA led to producing calcium aluminate hydrate formation. The strength development of the RAP-FA geopolymer occurred resulted from the polymerization reaction. The TCLP results demonstrate there is no environmental risk of these stabilized materials. Furthermore, FA based geopolymer can reduce the leachability of heavy metal in the RAP-FA blend.

Keywords: recycled asphalt pavement, geopolymer, heavy metal, microstructure

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Authors: Abdelmaoula Mahamoud Tahir, Sedat Sert

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The possibility of improving the shear strength of unsaturated clayey soil with the addition of olivine was investigated in this paper. Unconsolidated undrained triaxial tests (UU), under different cell pressures (namely: 100 kPa and 200 kPa), with varying percentages of olivine (10% and 20% by weight) and with one day, 28 days, and 56 days curing times, were performed to determine the shear strength of the soil. The increase in strength was observed as a function of the increase in olivine content. An olivine content of 25% was determined as the optimum value to achieve the targeted improvement for both cure times. A comparative study was also conducted between clay samples treated with only olivine and others in the presence of potassium hydroxide (KOH). Clay samples treated with olivine and activated with potassium hydroxide (KOH) had higher shear strength than non-activated olivine-treated samples. It was determined that the strength of the clay samples treated with only olivine did not increase over time and added resistance only with the high specific gravity of olivine. On the other hand, the samples activated with potassium hydroxide (KOH) added to the resistance with high specific gravity and the chemical bonds of olivine. Morphological and mineralogical analyzes were carried out in this study to see and analyze the chemical bonds formed after the reaction. The main components of this improvement were the formation of magnesium-aluminate-hydrate and magnesium-silicate-hydrate. Compared to older methods such as cement addition, these results show that in stabilizing clayey soils, olivine additive offers an energy-efficient alternative for reducing carbon dioxide emissions.

Keywords: ground stabilization, clay, olivine additive, KOH, microstructure

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Authors: Ratnakumar V. Kappagantula, Gordon D. Ingram, Hari B. Vuthaluru

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This paper analyzes a three reactor chemical looping process for hydrogen production from natural gas, allowing for carbon dioxide capture through chemical looping technology. An oxygen carrier is circulated to separate carbon dioxide, to reduce steam for hydrogen production and to supply oxygen for combustion. In this study, the emphasis is placed on the steam conversion in the steam reactor by investigating the hydrogen efficiencies of the complete system at steam conversions of 15.8% and 50%. An Aspen Plus model was developed for a Three Reactor Chemical Looping process to study the effects of operational parameters on hydrogen production is investigated. Maximum hydrogen production was observed under stoichiometric conditions. Different conversions in the steam reactor, which was modelled as a Gibbs reactor, were found when Gibbs-identified products and user identified products were chosen. Simulations were performed for different oxygen carriers, which consist of an active metal oxide on an inert support material. For the same metal oxide mass flowrate, the fuel reactor temperature decreased for different support materials in the order: aluminum oxide (Al2O3) > magnesium aluminate (MgAl2O4) > zirconia (ZrO2). To achieve the same fuel reactor temperature for the same oxide mass flow rate, the inert mass fraction was found to be 0.825 for ZrO2, 0.7 for MgAl2O4 and 0.6 for Al2O3. The effect of poisoning of the oxygen carrier was also analyzed. With 3000 ppm sulfur-based impurities in the feed gas, the hydrogen product energy rate of the process were found to decrease by 0.4%.

Keywords: aspen plus, chemical looping combustion, inert support balls, oxygen carrier

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Authors: Vinu Viswanath, Lawrence Dsouza, Ugo Ravon

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Syngas typically and intermediary gas product has a wide range of application of producing various chemical products, such as mixed alcohols, hydrogen, ammonia, Fischer-Tropsch products methanol, ethanol, aldehydes, alcohols, etc. There are several technologies available for the syngas production. An alternative to the conventional processes an attractive route of utilizing carbon dioxide and methane in equimolar ratio to generate syngas of ratio close to one has been developed which is also termed as Dry Reforming of Methane technology. It also gives the privilege to utilize the greenhouse gases like CO2 and CH4. The dry reforming process is highly endothermic, and indeed, ΔG becomes negative if the temperature is higher than 900K and practically, the reaction occurs at 1000-1100K. At this temperature, the sintering of the metal particle is happening that deactivate the catalyst. However, by using this strategy, the methane is just partially oxidized, and some cokes deposition occurs that causing the catalyst deactivation. The current research work was focused to mitigate the main challenges of dry reforming process such coke deposition, and metal sintering at high temperature.To achieve these objectives, we employed three different strategies of catalyst development. 1) Use of bulk catalysts such as olivine and pyrochlore type materials. 2) Use of metal doped support materials, like spinel and clay type material. 3) Use of core-shell model catalyst. In this approach, a thin layer (shell) of redox metal oxide is deposited over the MgAl2O4 /Al2O3 based support material (core). For the core-shell approach, an active metal is been deposited on the surface of the shell. The shell structure formed is a doped metal oxide that can undergo reduction and oxidation reactions (redox), and the core is an alkaline earth aluminate having a high affinity towards carbon dioxide. In the case of metal-doped support catalyst, the enhanced redox properties of doped CeO2 oxide and CO2 affinity property of alkaline earth aluminates collectively helps to overcome coke formation. For all of the mentioned three strategies, a systematic screening of the metals is carried out to optimize the efficiency of the catalyst. To evaluate the performance of them, the activity and stability test were carried out under reaction conditions of temperature ranging from 650 to 850 ̊C and an operating pressure ranging from 1 to 20 bar. The result generated infers that the core-shell model catalyst showed high activity and better stable DR catalysts under atmospheric as well as high-pressure conditions. In this presentation, we will show the results related to the strategy.

Keywords: carbon dioxide, dry reforming, supports, core shell catalyst

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Authors: E. Poupelloz, S. Gauffinet

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Ettringite Ca₆Al₂(SO₄)₃(OH)₁₂26H₂O is one of the major hydrates formed during cement hydration. Ettringite forms in Portland cement from the reaction between tricalcium aluminate Ca₃Al₂O₆ and calcium sulfate. Ettringite is also present in calcium sulfoaluminate cement in which it is the major hydrate, formed by the reaction between yeelimite Ca₄(AlO₂)₆SO₄ and calcium sulfate. About the formation of ettringite, numerous results are available in the literature even if some issues are still under discussion. However, almost all published work about ettringite was done on cementitious systems. Yet in cement, hydration reactions are very complex, the result of dissolution-precipitation processes and are submitted to various interactions. Understanding the formation process of a phase alone, here ettringite, is the first step to later understand the much more complex reactions happening in cement. This study is crucial for the comprehension of early cement hydration and physical behavior. Indeed formation of hydrates, in particular, ettringite, will have an influence on the rheological properties of the cement paste and on the need for admixtures. To make progress toward the understanding of existing phenomena, a specific study of nucleation and growth processes of ettringite was conducted. First ettringite nucleation was studied in ionic aqueous solutions, with controlled but different experimental conditions, as different supersaturation degrees (β), different pH or presence of exogenous ions. Through induction time measurements, interfacial ettringite crystals solution energies (γ) were determined. Growth of ettringite in supersaturated solutions was also studied through chain crystallization reactions. Specific BET surface area measurements and Scanning Electron Microscopy observations seemed to prove that growth process is favored over the nucleation process when ettringite crystals are initially present in a solution with a low supersaturation degree. The influence of stirring on ettringite formation was also investigated. Observation was made that intensity and nature of stirring have a high influence on the size of ettringite needles formed. Needle sizes vary from less than 10µm long depending on the stirring to almost 100µm long without any stirring. During all previously mentioned experiments, initially present ions are consumed to form ettringite in such a way that the supersaturation degree with regard to ettringite is decreasing over time. To avoid this phenomenon a device compensating the drop of ion concentrations by adding some more solutions, and therefore always have constant ionic concentrations, was used. This constant β recreates the conditions of the beginning of cement paste hydration, when the dissolution of solid reagents compensates the consumption of ions to form hydrates. This device allowed the determination of the ettringite precipitation rate as a function of the supersaturation degree β. Taking samples at different time during ettringite precipitation and doing BET measurements allowed the determination of the interfacial growth rate of ettringite in m²/s. This work will lead to a better understanding and control of ettringite formation alone and thus during cements hydration. This study will also ultimately define the impact of ettringite formation process on the rheology of cement pastes at early age, which is a crucial parameter from a practical point of view.

Keywords: cement hydration, ettringite, morphology of crystals, nucleation-growth process

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