Durability of geopolymer materials in sodium and magnesium sulfate solutions

This paper presents an investigation into the durability of geopolymer materials manufactured using class F fly ash and alkaline activators when exposed to a sulfate environment. Three tests were used to determine resistance of geopolymer materials. The tests involved immersions for a period of 5 months into 5% solutions of sodium sulfate and magnesium sulfate, and a solution of 5% sodium sulfate+5% magnesium sulfate. The evolution of weight, compressive strength, products of degradation and microstructural changes were studied.In the sodium sulfate solution, significant fluctuations of strength occurred with strength reduction 18% in the 8FASS material prepared with sodium silicate and 65% in the 8FAK material prepared with a mixture of sodium hydroxide and potassium hydroxide as activators, while 4% strength increase was measured in the 8FA specimens activated by sodium hydroxide. In the magnesium sulfate solution, 12% and 35% strength increase was measured in the 8FA and 8FAK specimens, respectively; and 24% strength decline was measured in the 8FASS samples. The most significant deterioration was observed in the sodium sulfate solution and it appeared to be connected to migration of alkalies into solution. In the magnesium sulfate solution, migration of alkalies into the solution and diffusion of magnesium and calcium to the subsurface areas was observed in the specimens prepared using sodium silicate and a mixture of sodium and potassium hydroxides as activators. The least strength changes were found in the solution of 5% sodium sulfate+5% magnesium sulfate. The material prepared using sodium hydroxide had the best performance, which was attributed to its stable cross-linked aluminosilicate polymer structure.     

Geopolymeric materials prepared using Class F fly ash and elevated temperature curing

This paper reports the results of the study of the influence of elevated temperature curing on phase composition, microstructure and strength development in geopolymer materials prepared using Class F fly ash and sodium silicate and sodium hydroxide solutions. In particular, the effect of storage at room temperature before the application of heat on strength development and phase composition was studied. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and SEM were utilised in this study.Long precuring at room temperature before application of heat was beneficial for strength development in all studied materials, as strength comparable to 1 month of curing at elevated temperature can develop in this case only after 24 h of heat curing. The main product of reaction in the geopolymeric materials was amorphous alkali aluminosilicate gel. However, in the case of sodium hydroxide activator in addition to it, traces of chabazite, Linde Type A, Na-P1 (gismondine) zeolites and hydroxysodalite were also present. The type of zeolite present and composition of aluminosilicate gel were dependent on the curing history.     

Synthesis of heat and ambient cured one-part geopolymer mixes with different grades of sodium silicate

The use of solid activators in the manufacture of geopolymer enhances its commercial viability as it aids the development of a one-part “just add water” geopolymer mixture, similar to the conventional Portland cement-based materials. This study is aimed to synthesize heat and ambient cured one-part geopolymer mixes. Appropriate combinations of low calcium (Class F) fly ash, slag and hydrated lime as the aluminosilicate source materials were activated by three different grades of sodium silicate and a combination of sodium silicate and sodium hydroxide powders. A conventional two-part geopolymer mix with the commonly used sodium hydroxide and sodium silicate solutions was also made for comparison. Effects of the type and amount of the solid activator, the amount of fly ash replacement with slag and hydrated lime and water content on short term mechanical properties of the heat cured one-part geopolymer mixtures including workability of the fresh mix, hardened density and compressive strength were evaluated. Subsequently, effects of ambient curing on the properties of the developed one-part geopolymer mixes were also investigated. Moderate to high compressive strength of over 37 MPa developed for the heat and ambient cured one-part geopolymer mixes. The 28-days compressive strengths of the ambient cured one-part geopolymer mixtures, regardless of the type of activator and geopolymer source materials, were comparable to those of the counterpart heat cured one-part geopolymer mixes. Such one-part geopolymer mixes could enhance the commercial viability and large-scale applications of the geopolymer in the construction industry.     

室温碱激发低钙粉煤灰地质聚合物配比试验研究

为得到室温下粉煤灰与碱激发剂质量比、水玻璃与氢氧化钠溶液质量比和氢氧化钠溶液摩尔浓度对粉煤灰地质聚合物力学性能的影响,以低钙粉煤灰为原料,制备了地质聚合物胶凝材料。采用正交试验方法,分析粉煤灰地质聚合物抗压强度,探讨碱激发剂配比对粉煤灰地质聚合物力学性能的影响,结合SEM、XRD和FTIR对试样进行表征,并对该材料的应力-应变曲线进行了研究。结果表明:粉煤灰地质聚合物的抗压强度随着激发剂掺量的减少而增大,水玻璃在激发剂中的比值与粉煤灰地质聚合物的抗压强度呈现正相关,其中粉煤灰与碱激发剂质量比为1.8,水玻璃与氢氧化钠溶液质量比为2.5且氢氧化钠溶液的浓度为10 mol/L时,120 d龄期的抗压强度可达51.98 MPa。对应力-应变曲线分析得出,在一定程度上,激发剂的掺入量对粉煤灰地质聚合物的破坏应变和弹性模量有较大影响。SEM、XRD和FTIR分析表明随着养护时间增长,胶凝材料体系内结构更致密,生成了更多的硅铝酸盐凝胶。     

Fibre-reinforced boroaluminosilicate geopolymers: A comparative study

This paper investigates the effect of fibres on the physical and mechanical behaviour of boroaluminosilicate geopolymers (BASG) compared to conventional aluminosilicate binders. The use of various types of fibres by the means of reinforcing geopolymers against flexural loads is very common. In this work, fly ash and ground granulated blast furnace slag (GGBS) are utilised as raw materials to generate geopolymer specimens. Different alkaline solutions comprising sodium hydroxide, sodium silicate, and borax are prepared to activate precursors. The sodium silicate solution is substituted with borax by 30?wt% and 70?wt% in order to produce fly ash and slag-based BASG respectively. Steel and polymer fibres are employed in the mixtures for reinforcement. Three-point bending and mini slump tests are conducted for assessing the flexural strength, elastic modulus, toughness, and flow of geopolymer specimens. A pair plotting interpretation is also used in order to illustrate the patterns. The obtained results indicate that the fly ash-based BASG mortar shows superior flexural strength to the GGBS-based BASG mortar. The flexural strength of fly ash-made aluminosilicate geopolymer declines from 7.3?MPa to 6.4?MPa with an increase in the content of steel fibres from 1% to 2%. Inversely, raising the percentage of steel fibres in the fly ash-based BASG mortar caused a slight growth in the flexural strength of specimens. The polypropylene fibres, when added sufficiently, play a significant role in improving the toughness of fly ash-based BASG and slag-based aluminosilicate mixtures, more than 0.8 and 0.7?J surge in the toughness respectively. In addition, the polypropylene and steel fibres perform well in improving the elastic modulus of slag-based BASG and fly ash-based aluminosilicate binders. While keeping the water to binder ratio constant, introducing the steel fibre increased the flow of fly ash-based geopolymers. Nonetheless, the polymer fibres declined the flow of mortars.     

激发剂对赤泥地聚物砂浆力学性能的影响

以热活化氧化铝赤泥为主要原料制备赤泥地聚物砂浆,对比研究了激发剂种类和掺量对赤泥地聚物力学性能的影响及其合成机理。结果表明,水玻璃、石灰-碱（质量比为2∶1）、石膏-碱（质量比为2∶1）均能改善氧化铝赤泥的反应活性,促进赤泥地聚物的合成,其中水玻璃（氧化硅与氧化钠物质的量比为1.5）的改性效果最为显著。水玻璃、石灰-碱、石膏-碱的最佳掺量分别为20%、7%、10%。水玻璃掺量为20%时,赤泥地聚物砂浆28 d抗压强度和28 d抗折强度分别为32.1 MPa和6.0 MPa。改变激发剂的种类和掺量,可以调整赤泥地聚物砂浆体系的碱度,改变铝硅酸结构的解聚和地聚物的缩聚过程,从而影响其力学性能。     

矿粉掺量对偏高岭土基地聚合物性能和结构影响

以高炉矿渣、偏高岭土、水玻璃和氢氧化钠为主要原料,制备矿粉-偏高岭土体系地聚合物。通过调节矿粉掺量(0%~50%范围内),研究钙组分含量对地聚合物抗压强度、凝结时间、物相组成和微观结构的影响。结果表明:当矿粉掺量为30%时,地聚合物样品310 min初凝,395 min终凝,1、3、7和28 d抗压强度分别达到52.8、73.9、87.1和102.3 MPa,达到快凝、早强和高强的目的。     

Alkali-activated waste ceramics: Importance of precursor particle size distribution

The waste ceramics belongs to wide range of aluminosilicate materials which can be alkaline-activated to geopolymer cement – possible “green” alternative to conventional Portland cement. The studied ceramic material is generated during the size adjustment of ceramic building blocks by means of grinding. It means that most of the material is very fine, but it contains also some larger shards. This ceramic powder was used as geopolymer precursor “as received” and after removal of particles retained on 1, 0.5 and 0.125 mm sieves. These four types of precursor were activated by sodium silicate (SiO₂/Na₂O = 1) solution. The prepared mortars were tested for strength, basic physical properties, transport parameters and characterized by help of XRD and thermal analysis. It was found that the best mechanical performance provided the precursor after removal of particles retained on 0.5 mm sieve thanks to the highest geopolymerization rate. The presence of coarser particles in precursor gave rise to porosity, what consequently influenced transport parameter of geopolymers towards the lower thermal conductivity and faster moisture transport.     

硅酸钠模数对无机聚合物力学性能与微观结构的影响

用模数m=1.0、1.2、1.4和1.6的4种硅酸钠溶液作激发剂制备偏高岭土基无机聚合物,通过强度测试、红外分析(IR)、X线衍射(XRD)和扫描电镜(SEM)等方法考察激发剂模数对无机聚合物力学性能和微观结构的影响。结果表明:模数在1.0~1.6变化时,激发剂中硅氧四面体呈低聚合态;随养护时间延长,无机聚合物抗压强度和抗折强度提高,m=1.2的无机聚合物28 d抗压强度最高(74.6 MPa),抗折强度为11.2 MPa;4种无机聚合物主体相均呈非晶态,结构上由凝胶体和残留原料颗粒组成,其中,m=1.2时无机聚合物的显微结构最平整。     

碱激发偏高岭土基地质聚合物的制备及抗压强度研究

为了响应“双碳”政策节能减排的号召,本文采用偏高岭土和高炉矿渣为原材料制备地质聚合物。以抗压强度为指标优化制备条件,探讨确定影响地质聚合物强度的因素。通过正交试验确定偏高岭土基地质聚合物的最佳配比,通过热重和XRD分析不同温度煅烧的偏高岭土组分。研究结果表明,在高岭土煅烧温度为800 ℃时,偏高岭土基地质聚合物的最佳配合比为氢氧化钠与硅酸钠的质量比为6.5∶1,激发剂的质量掺量为14.2%,其28 d抗压强度能达到46.6 MPa。偏高岭土基地质聚合物抗压强度随激发剂的掺量增加而增大,随氢氧化钠与硅酸钠的质量比的增大先增大后减小,随高岭土煅烧温度的升高先增大后减小。     

Thermal behaviour of geopolymers prepared using class F fly ash and elevated temperature curing

This article reports a study of thermal stability of properties upon firing at 800-1200 °C of geopolymer materials prepared using class F fly ash and Na and K alkaline activators. Compressive strength and shrinkage measurements, XRD, SEM (BEI), TGA and MIP were utilised in these studies. The materials were prepared at water/binder ratios in a range of 0.09-0.35, using compaction pressures up to 10 MPa and curing temperatures 80 and 100 °C. Thermal stability of the studied geopolymer materials was rather low. In the samples prepared using sodium-containing activators rapid deterioration of strength at 800 °C was observed, which was connected to a dramatic increase of the average pore size. Initially amorphous structures were replaced by the crystalline Na-feldspars. In materials prepared using fly ash and potassium silicate compressive strength was significantly increased on heating, deterioration of strength started at 1000 °C. After firing these materials remained amorphous with reduced average pore size and significantly increased compressive strength. Compaction at 1-10 MPa reduced shrinkage on firing in all materials. Geopolymer materials prepared using class F fly ash and alkaline activators showed high shrinkage as well as large changes in compressive strength with increasing fired temperature in the range of 800-1200 °C. Thus the materials were found unsuitable for refractory insulation applications.     

Effect of nano silica and fine silica sand on compressive strength of sodium and potassium activators synthesised fly ash geopolymer at elevated temperatures

Environment friendly geopolymer is a new binder which gained increased popularity due to its better mechanical properties, durability, chemical resistance, and fire resistance. This paper presents the effect of nano silica and fine silica sand on residual compressive strength of sodium and potassium based activators synthesised fly ash geopolymer at elevated temperatures. Six different series of both sodium and potassium activators synthesised geopolymer were cast using partial replacement of fly ash with 1%, 2%, and 4% nano silica and 5%, 10%, and 20% fine silica sand. The samples were heated at 200°C, 400°C, 600°C, and 800°C at a heating rate 5°C per minute, and the residual compressive strength, volumetric shrinkage, mass loss, and cracking behaviour of each series of samples are also measured in this paper. Results show that, among 3 different NS contents, the 2% nano silica by wt. exhibited the highest residual compressive strength at all temperatures in both sodium and potassium‐based activators synthetised geopolymer. The measured mass loss and volumetric shrinkage are also lowest in both geopolymers containing 2% nano silica among all nano silica contents. Results also show that although the unexposed compressive strength of potassium‐based geopolymer containing nano silica is lower than its sodium‐based counterpart, the rate of increase of residual compressive strength exposed to elevated temperatures up to 400°C of potassium‐based geopolymer containing nano silica is much higher. It is also observed that the measured residual compressive strengths of potassium based geopolymer containing nano silica exposed at all temperatures up to 800°C are higher than unexposed compressive strength, which was not the case in its sodium‐based counterpart. However, in the case of geopolymer containing fine silica sand, an opposite phenomenon is observed, and 10% fine silica sand is found to be the optimum content with some deviations. Quantitative X‐ray diffraction analysis also shows higher amorphous content in both geopolymers containing nano silica at elevated temperatures than those containing fine silica sand.     

Influence of Aluminosilicate for the Prediction of Mechanical Properties of Geopolymer Concrete – Artificial Neural Network

In this paper, details and results of experimental and predictive studies carried out to determine the mechanical properties of Aluminosilicate materials like Ground Granulated Blast furnace Slag (GGBS) and Fly Ash (FA) based geopolymer concrete specimens are presented and discussed. The major parameters considered in the experimental study are the percentages of GGBS and Fly ash and the percentage of manufactured sand (m-sand) used to replace conventional river sand used in the production of geopolymer concrete. Sodium hydroxide and sodium silicate solutions were used as the activator in the production of geopolymer concrete. The mechanical properties of the geopolymer concrete determined were the compressive strength, split-tensile strength and flexural strength. The test results showed that the mechanical properties of geopolymer concrete improved with increase in the percentage use of GGBS. Also, it was observed from the test results that increase in the percentage use of m-sand increased the mechanical properties of the geopolymer concrete up to an optimum dosage beyond which reduction in the mechanical properties was observed. The predicted mechanical properties of the geopolymer concrete using Artificial Neural Network (ANN) was found to be in good agreement with the test results.

     

地聚物橡胶混凝土的力学、抗冲击性能及强度机理分析

为探究橡胶再生集料在地聚物混凝土中的增韧作用,采用不同比例的橡胶再生集料(粒径为0.15~0.3 mm和1~4 mm)代替地聚物混凝土中的普通集料。首先,采用工业废渣中粒化高炉矿渣粉为原料,水玻璃溶液和NaOH为激发剂制备地聚物胶凝材料,并与普通集料、橡胶再生集料混合制备地聚物橡胶混凝土;然后对地聚物橡胶混凝土的力学性能、抗冲击性能和强度机理进行探究。结果表明:添加适量比例的橡胶再生集料可提高地聚物混凝土的抗压强度,增幅为5%左右,这与橡胶再生集料表面在NaOH碱环境中的氧化和降解作用有关;但地聚物橡胶混凝土在劈裂荷载和弯曲荷载下易断裂,劈裂抗拉强度和抗折强度降低20%~30%,这是地聚物橡胶混凝土的典型特点。通过落锤冲击试验和弯拉冲击试验可知,橡胶再生集料能大幅提高地聚物混凝土的抗冲击性能,最高增幅超过200%。这是由于橡胶再生集料具有的柔性和弹性特征吸收了部分冲击能量,同时延缓了冲击荷载下混凝土初始开裂到失效破坏过程,减少了裂缝开裂应力集中,提高了地聚物混凝土的延性。在地聚物碱性条件下,橡胶颗粒表面发生氧化和降解作用,表面变得粗糙,与地聚物基体结合紧密;橡胶表面在NaOH作用下,产生羟基、羧基等亲水基团,有利于水化产物在橡胶再生集料表面附着。     

地质聚合物激发剂及其激发原理

激发剂在制备地质聚合物的过程中发挥着重要的作用。首先概述了酸、碱和盐3类激发剂及其激发效果,通过介绍氢氧化钠、氢氧化钾和水玻璃等常用碱激发剂的激发效果,具体分析各类碱激发剂的作用差别。阐述了乙酸、盐酸、硫酸和磷酸等典型的酸激发剂的研究进展,以及硫酸盐、硅酸盐和铝酸盐等作为盐类激发剂的活化能力,在此基础上对3类激发剂的优缺点进行了总结分析。同时通过论述酸、碱和盐3类激发剂的激发原理,进一步表明了3类激发剂都具备激发地聚物原料活性的能力,都能够不同程度地加快地聚体系水化反应进程,显著提高地聚体系的强度。最后,对激发剂在地聚物领域的未来发展作出了展望。     

粉煤灰基地聚合物无机涂料的制备与性能

以低钙型粉煤灰为主要原料,硅酸钠和氢氧化钠为复合碱激发剂,硅烷偶联剂(KH550)为增强材料,硅丙乳液为辅助成膜物质制备地聚合物无机涂料。研究了硅烷偶联剂掺量、反应温度以及水固比对地聚合物无机涂料的成膜性、耐水性和耐洗刷性等性能的影响,并通过XRD、FTIR、SEM、TG-DSC分析了无机涂料的微观结构及其耐高温性能。结果表明,当制备温度为60 ℃、水固比为0.31(质量比)、硅烷偶联剂掺量为3.6%(质量分数)时,地聚合物无机涂料在室温下的成膜性良好,无开裂现象,涂料24 h内质量吸水率为1.84%,耐洗刷性可达12 000次,7 d时硬度为154 s。地聚合物无机涂层内部主要是无定形的硅铝酸盐凝胶,硅烷偶联剂经水解、键合生成簇状产物填充在涂层的孔隙之间,增加了涂层的密实性,抑制了裂纹的产生。涂层在25~800 ℃的失重率为12.0%~13.0%,未发现明显的地聚合物热分解现象,说明涂层耐高温性能良好。     

Mechanical and microstructural evolutions of fly ash/slag-based geopolymer at high temperatures: Effect of curing conditions

Designing a building material with excellent heat resistance is crucial for protection against catastrophic fires. Geopolymer materials have been investigated as they offer better heat resistance than traditional cement owing to their ceramic-like properties. Curing temperature and conditions are crucial factors that determine the properties of geopolymers, but their impacts on the heat resistance of geopolymers remain unclear. This study produced geopolymers from fly ash and ground granulated blast furnace slag by using sodium silicate and sodium hydroxide solutions as alkaline solutions. To examine the effect of curing conditions on the high-temperature performance of geopolymer, four different curing conditions, namely, heat curing (70 °C for 24 h), ambient curing (20 °C), water curing, and the combination of heat and water curing (70 °C for 24 h followed by water curing), were applied. At 28 d, the specimens were subjected to high temperatures (500 °C, 750 °C, and 950 °C), and their mechanical and microstructural evolutions were studied. The results revealed that the curing condition significantly affects the properties of the unexposed geopolymer; the effect on its high-temperature performance is insignificant. Furthermore, all the specimens could maintain adequate compressive strength after exposure to the maximum temperature of 950 °C, promising the use of geopolymer for structural applications.     

Influence of new organic alkali activators on microstructure and strength of fly ash geopolymer

The fly ash geopolymer with improved mechanical properties was prepared by a new mixture alkali activator. In this paper, sodium tert-butanol, an organic strong alkali was used as an activator for preparing fly ash geopolymer to improve their mechanical properties. The effect of activator content and type on the macroscopic level of fly ash geopolymer was investigated experimentally by three types of activators: sodium tert-butanol, sodium silicate, and sodium tert-butoxide/sodium silicate mix activator. The microstructure of the fly ash geopolymer was characterized by ATR-FTIR, SEM-EDS, XRD, and Brunauer-Emmett-Teller (BET) physical adsorption method. The results showed that the new mixture alkali activator prepared by 5% sodium tert-butoxide and 10% sodium silicate improved the denseness and integrity of the microstructure of the fly ash geopolymer. Consequently, the mechanical properties of fly ash geopolymer are improved. The microscopic results demonstrated that the C–OH in tert-butanol after the hydrolysis of sodium tert-butoxide and Si–OH in the geopolymer can form C–O–Si bonds, forming a more complex three-dimensional network structure. This paper reveals the enhancement mechanism of organic alkali as activators for preparing fly ash geopolymer, and provides support for the subsequent development of organic strong alkali activators.     

NaOH-activated ground fly ash geopolymer cured at ambient temperature

NaOH-activated ground fly ash geopolymers, cured at room temperature, were studied in this paper. Ground fly ash (GFA), with a median particle size of 10.5 μm, was used as source material. NaOH concentrations of 4.5-16.5 M (M) were used as an alkali activator. Compressive strength tests and microstructure observations using SEM, EDX, XRD and FTIR were performed. Results indicated that GFA gave higher strength geopolymer paste compared to original fly ash. Ground fly ash could be used as a source material for making geopolymers cured at room temperature. An increase in NaOH concentration from 4.5 to 14.0 M increased the strength of GFA geopolymer pastes. Microstructure studies indicated that NaOH concentrations of 12.0-14.0 M created new crystalline products of sodium aluminosilicate. The compressive strengths at 28 days of 20.0-23.0 MPa were obtained with the NaOH concentrations of 9.5-14.0 M. Increasing the NaOH concentration beyond this point resulted in a decrease in the strength of the paste due to early precipitation of aluminosilicate products.     

Fly Ash Porous Material using Geopolymerization Process for High Temperature Exposure

This paper presents the results of a study on the effect of temperature on geopolymers manufactured using pozzolanic materials (fly ash). In this paper, we report on our investigation of the performance of porous geopolymers made with fly ash after exposure to temperatures from 600 °C up to 1000 °C. The research methodology consisted of pozzolanic materials (fly ash) synthesized with a mixture of sodium hydroxide and sodium silicate solution as an alkaline activator. Foaming agent solution was added to geopolymer paste. The geopolymer paste samples were cured at 60 °C for one day and the geopolymers samples were sintered from 600 °C to 1000 °C to evaluate strength loss due to thermal damage. We also studied their phase formation and microstructure. The heated geopolymers samples were tested by compressive strength after three days. The results showed that the porous geopolymers exhibited strength increases after temperature exposure.