碱矿渣水泥石碳化行为及机理研究
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摘要
碱矿渣水泥是环境友好型绿色胶凝材料,使用性能优异,生产过程能有效利用工业副产品和废渣,生产工艺简单,生产能耗低,自然资源消耗和温室气体排放少,被誉为二十一世纪最具开发潜力的胶凝材料。从应用的角度,提高材料耐久性是延长结构使用寿命、促进社会经济可持续发展的需要。业已证明,碳化与钢筋锈蚀是混凝土结构耐久性破坏的主要类型。虽然碱矿渣混凝土具有一系列优良性能,但已有研究表明,其碳化速率较高,特别是强度等级较低的混凝土,表现尤为突出。不仅如此,总体而言,有关碱矿渣混凝土的抗碳化性能研究极少,对其抗碳化性能的评价存在争议,对其碳化行为的内在本质没有统一认识,有效改善与提高其抗碳化能力的技术途径尚未确立,上述问题是该材料研究的薄弱环节,也是制约其应用发展的关键技术问题之一。因此,研究碱矿渣水泥石(AASS)的碳化行为与微观机理,对科学评价碱矿渣混凝土的抗碳化能力,指导碱矿渣混凝土结构的耐久性设计与应用发展均具有重要意义。
论文以水玻璃与NaOH为碱组分制备的碱矿渣水泥石为对象,研究了碱组分种类、碱当量、水玻璃模数、水胶比、养护条件及碳化前处理方式对该水泥石碳化程度与收缩行为的影响,分析了碳化对碱矿渣水泥石孔溶液pH值及Na~+、K~+、Ca~(2+)含量的影响;采用X-射线衍射(XRD)、扫描电子电镜(SEM )、综合热分析(TG-DSC)及傅立叶转换红外光谱分析(FT-IR)等测试手段,研究了碱矿渣水泥石的碳化产物与微观结构,结合氮吸附方法分析了碳化对碱矿渣水泥石孔结构的影响;通过提高固态分散相碱度、降低水泥石干燥收缩与水泥石可溶性碱含量等技术措施,研究了改善碱矿渣水泥石抗碳化性能的技术途径。研究揭示的主要规律与取得的主要成果概括如下:
在3%~6%范围内,碱矿渣水泥石的碳化程度随碱当量提高而减小,但减小的程度随碱当量的提高而减弱。同一碱当量水平,NaOH为碱组分的碱矿渣水泥石碳化程度大于水玻璃为碱组分的碱矿渣水泥石。在1.0~2.0范围内,随模数增加,水玻璃为碱组分的碱矿渣水泥石碳化程度先减小,后增大。碱当量为4%~6%、模数为1.2~1.5时,碱矿渣水泥石具有良好抗碳化能力。此外,碱矿渣水泥石碳化程度随水胶比提高而增加,随碳化前养护龄期延长而降低。水中养护的碱矿渣水泥石碳化程度大于同龄期标准养护的碱矿渣水泥石。
相同水胶比时,碱矿渣水泥砂浆碳化程度大于硅酸盐水泥砂浆。相同扩展度时,碱矿渣水泥砂浆的碳化程度小于硅酸盐水泥砂浆。碳化后,硅酸盐水泥砂浆抗压强度有所提高,在碳化龄期60d内,碱矿渣水泥砂浆抗压强度随碳化龄期延长呈降低趋势。
碱矿渣水泥石碳化收缩特征研究表明,碳化没有引起水泥石收缩的增加。在3%~6%范围内,碱矿渣水泥石碳化收缩随碱当量提高而减小。模数为1.2~1.5的水玻璃所配水泥石的碳化收缩较小。在0.30~0.35范围内,碱矿渣水泥石碳化收缩随水胶比提高而增大。随碳化前养护龄期延长,碳化收缩减小。水中养护的碱矿渣水泥石碳化收缩大于同龄期标准养护的水泥石。
碳化前,碱矿渣水泥石孔溶液Na~+含量较多,K~+含量较少,而Ca~(2+)含量很低,NaOH为碱组分的水泥石孔溶液pH值大于水玻璃为碱组分的水泥石。碳化60d时,水泥石孔溶液pH值降低至10左右,Na~+含量增加,K~+与Ca~(2+)含量减少。水胶比为0.30,模数1.2的水玻璃配制的碱矿渣水泥石主要含孔径小于20nm的孔,体积百分率可达78%,NaOH配制的碱矿渣水泥石中,孔径大于20nm的毛细孔较多,体积百分率可达68%。碳化使碱矿渣水泥石比表面积增加、平均孔径、最可几孔径减小。碱矿渣水泥石的C-S-H凝胶是较接近托贝莫来石的水化硅酸钙,水玻璃为碱组分的碱矿渣水泥石的C-S-H凝胶C/S小于NaOH为碱组分的碱矿渣水泥石。碳化引起C-S-H凝胶脱钙,使C-S-H凝胶C/S降低,聚合度增加。碳化产物CaCO_3的存在形式主要为方解石,随碳化龄期延长,出现球霰石与文石。另外,碳化还会形成单斜钠钙石(Na_2CO_3·CaCO_3·5H_2O)与苏打石(NaHCO_3)。碱矿渣水泥石孔溶液的高碱性、水化产物不存在Ca(OH)_2、干燥收缩较大是其碳化比较严重的主要原因。
碱组分不同,改善碱矿渣水泥石抗碳化性能的技术途径不同。水玻璃为碱组分的碱矿渣水泥石,提高固态分散相碱度比较适用,掺入适量Ca(OH)_2、Ba(OH)2与ZnCl_2能有效降低水泥石碳化程度;NaOH为碱组分的碱矿渣水泥石,降低水泥石干燥收缩比较适用,掺入适量引气剂与Na2SO4能有效降低碱矿渣水泥石碳化程度。
Alkali-activated slag cement is a kind of environmental friendly green binding material, which has the advantages of superior properties, effective utilization of industrial by-products, simple producing progress, low energy, low natural resource consuming and greenhouse gases emission. So it is praised as one of most exploration potential cementitious materials in the 21st century. From the practical application angle, improving the durability of materials can adapt well to extend service time of concrete structures and to the sustainable development of soc-economy. Carbonation and steel corrosion has been proven to be the main form of damages to the concrete structures durability. Although alkali-activated slag concrete has noticeable excellent properties, previous studies have demonstrated that its carbonation rate is high, which especially be reflected in the low strength grade concrete. Overall,there is little study on its carbonation resistance and there is dispute on its carbonation resistance evaluation, there is no common agreement on the essence of carbonation behavior and the proper technical approach to improve the carbonation resistance of alkali-activated slag concrete has not been established, which is the weak link and is one of the key technologies to restrict its development. Therefore, the investigation of carbonation behaviour and microscopic mechanism of alkali-activated slag cement stone(AASS) would lay a foundation to scientifically evaluate the ability of alkali-activated slag concrete to carbonation resistance and to guide the durability design and the application and development of alkali-activated slag concrete structure.
In this project, alkali-activated slag cement stone(AASS) activated by water glass and NaOH was used to investigate the effect of main factors such as alkali activator type, Na_2O equivalent, water glass module(Ms), water binder ratio(W/B), curing condition and pretreatment method on the carbonation depth and shrinkage behavior. The effect of carbonation on the pH value, Na~+, K~+ and Ca~(2+) content of pore solution of AASS was also studied. The products of carbonation and their microscopic structure were identified by using XRD, SEM, TG-DSC, FT-IR analysis and so on. The effect of carbonation on the pore structure of AASS was analysed by using nitrogen absorption measurement. Based on the technical measures of increasing the alkalinity of solid dispersive phase and reducing the drying shrinkage and soluble alkali content of AASS, technical approach to improve the carbonation resistance of AASS was studed. Chief laws and results are summarized as follows:
In the range of 3%～6%, carbonation depth of AASS decreases with the increase of Na2O equivalent, although the extent of reduction decreases with the increase of Na2O equivalent. At the same Na2O equivalent, the carbonation depth of AASS activated by NaOH is larger than that of AASS activated by water glass. In the range of 1.0～2.0, with the increase of module, carbonation depth of AASS activated by water glass first decreases, then followed by an increase. When Na2O equivalent is 4%~6% and the module of water glass is 1.2~1.5, AASS possesses excellent capability to carbonation resistance. Besides, carbonation depth of AASS increases when W/B increases and decreases when standard curing ages extends. Water curing can increase the carbonation depth of AASS.
Alkali-activated slag cement mortar is more easily carbonated than Portland cement mortars when water-binder ratio is the same. While the consistency of mortars is the same, alkali-activated slag cement mortar used water glass as alkali activator is less carbonated than Portland cement mortar. After being carbonated, the compressive strength of Portland cement mortar increases, while that of alkali-activated slag cement mortar shows the tendency of decline with the increase of carbonation ages within 60 days.
The study on the characteristic of carbonation shrinkage of AASS shows that carbonation doesn’t increase the shrinkage of AASS. In the range of 3%～6%, carbonation shrinkage of AASS decreases with the increase of Na2O equivalent. When water glass is used as the activator, carbonation shrinkage is relatively small with the module of 1.2~1.5. In the range of 0.30～0.35, while W/B increases, carbonation shrinkage of AASS increases and that decreases when standard curing ages extends. Carbonation shrinkage of AASS under water curing is larger than that of standard curing at the same age.
Before carbonation, Na~+ content is more, K~+ content is less, while Ca~(2+) content is much lower in the pore solution of AASS. The pore solution pH value of AASS activated by NaOH is larger than that of AASS activated by water glass. After being 60d carbonated, pH value of pore solution reduces to about 10 and Na~+ content increases, while K~+ and Ca~(2+) content decreases.
When water binder ratio is 0.30, in the AASS activated with water glass, the diameter of main pores is less than 20 nm which volume percentage touches 78%. While in the AASS activated with NaOH, capillary which diameter more than 20nm is more and its volume percentage is 68%. Carbonation increases the amount of the specific surface area of AASS and reduces the average and the most probable distribution pore diameters. C-S-H gel of AASS is an amorphous gel which is more close to tobermorite. C/S ratio of C-S-H gel of AASS activated with water glass is smaller than that of AASS activated with NaOH. Carbonation causes decalcification of C-S-H gel ,so C/S ratio of C-S-H gel decreases, polymerization degree increases. As carbonation products, the main form of CaCO_3 is calcite. With the process of carbonation, vaterite and aragonite come into being. Besides, gaylussite and nahcolite have also been detected. The existence of more alkali (Na~+、K~+) in the pore solution, no existence of Ca(OH)_2 crystal in hydration product and the larger drying shrinkage of alkali- activated slag cement stone are the important reason for its serious carbonation.
Alkali-activated slag cement stone with different activator has its own proper technical approach to improve the carbonation resistance. Increasing the alkalinity of solid dispersive phase is suitable for AASS activated with water glass. Right amount of Ca(OH)_2,Ba(OH)2 and ZnCl_2 can effectively reduce the carbonation depth of AASS. While to AASS activated with NaOH, decrescence of drying shrinkage is useful. Right amount of air entraining agent and Na2SO4 do well to reduce the carbonation depth of AASS.
论文以水玻璃与NaOH为碱组分制备的碱矿渣水泥石为对象,研究了碱组分种类、碱当量、水玻璃模数、水胶比、养护条件及碳化前处理方式对该水泥石碳化程度与收缩行为的影响,分析了碳化对碱矿渣水泥石孔溶液pH值及Na~+、K~+、Ca~(2+)含量的影响;采用X-射线衍射(XRD)、扫描电子电镜(SEM )、综合热分析(TG-DSC)及傅立叶转换红外光谱分析(FT-IR)等测试手段,研究了碱矿渣水泥石的碳化产物与微观结构,结合氮吸附方法分析了碳化对碱矿渣水泥石孔结构的影响;通过提高固态分散相碱度、降低水泥石干燥收缩与水泥石可溶性碱含量等技术措施,研究了改善碱矿渣水泥石抗碳化性能的技术途径。研究揭示的主要规律与取得的主要成果概括如下:
在3%~6%范围内,碱矿渣水泥石的碳化程度随碱当量提高而减小,但减小的程度随碱当量的提高而减弱。同一碱当量水平,NaOH为碱组分的碱矿渣水泥石碳化程度大于水玻璃为碱组分的碱矿渣水泥石。在1.0~2.0范围内,随模数增加,水玻璃为碱组分的碱矿渣水泥石碳化程度先减小,后增大。碱当量为4%~6%、模数为1.2~1.5时,碱矿渣水泥石具有良好抗碳化能力。此外,碱矿渣水泥石碳化程度随水胶比提高而增加,随碳化前养护龄期延长而降低。水中养护的碱矿渣水泥石碳化程度大于同龄期标准养护的碱矿渣水泥石。
相同水胶比时,碱矿渣水泥砂浆碳化程度大于硅酸盐水泥砂浆。相同扩展度时,碱矿渣水泥砂浆的碳化程度小于硅酸盐水泥砂浆。碳化后,硅酸盐水泥砂浆抗压强度有所提高,在碳化龄期60d内,碱矿渣水泥砂浆抗压强度随碳化龄期延长呈降低趋势。
碱矿渣水泥石碳化收缩特征研究表明,碳化没有引起水泥石收缩的增加。在3%~6%范围内,碱矿渣水泥石碳化收缩随碱当量提高而减小。模数为1.2~1.5的水玻璃所配水泥石的碳化收缩较小。在0.30~0.35范围内,碱矿渣水泥石碳化收缩随水胶比提高而增大。随碳化前养护龄期延长,碳化收缩减小。水中养护的碱矿渣水泥石碳化收缩大于同龄期标准养护的水泥石。
碳化前,碱矿渣水泥石孔溶液Na~+含量较多,K~+含量较少,而Ca~(2+)含量很低,NaOH为碱组分的水泥石孔溶液pH值大于水玻璃为碱组分的水泥石。碳化60d时,水泥石孔溶液pH值降低至10左右,Na~+含量增加,K~+与Ca~(2+)含量减少。水胶比为0.30,模数1.2的水玻璃配制的碱矿渣水泥石主要含孔径小于20nm的孔,体积百分率可达78%,NaOH配制的碱矿渣水泥石中,孔径大于20nm的毛细孔较多,体积百分率可达68%。碳化使碱矿渣水泥石比表面积增加、平均孔径、最可几孔径减小。碱矿渣水泥石的C-S-H凝胶是较接近托贝莫来石的水化硅酸钙,水玻璃为碱组分的碱矿渣水泥石的C-S-H凝胶C/S小于NaOH为碱组分的碱矿渣水泥石。碳化引起C-S-H凝胶脱钙,使C-S-H凝胶C/S降低,聚合度增加。碳化产物CaCO_3的存在形式主要为方解石,随碳化龄期延长,出现球霰石与文石。另外,碳化还会形成单斜钠钙石(Na_2CO_3·CaCO_3·5H_2O)与苏打石(NaHCO_3)。碱矿渣水泥石孔溶液的高碱性、水化产物不存在Ca(OH)_2、干燥收缩较大是其碳化比较严重的主要原因。
碱组分不同,改善碱矿渣水泥石抗碳化性能的技术途径不同。水玻璃为碱组分的碱矿渣水泥石,提高固态分散相碱度比较适用,掺入适量Ca(OH)_2、Ba(OH)2与ZnCl_2能有效降低水泥石碳化程度;NaOH为碱组分的碱矿渣水泥石,降低水泥石干燥收缩比较适用,掺入适量引气剂与Na2SO4能有效降低碱矿渣水泥石碳化程度。
Alkali-activated slag cement is a kind of environmental friendly green binding material, which has the advantages of superior properties, effective utilization of industrial by-products, simple producing progress, low energy, low natural resource consuming and greenhouse gases emission. So it is praised as one of most exploration potential cementitious materials in the 21st century. From the practical application angle, improving the durability of materials can adapt well to extend service time of concrete structures and to the sustainable development of soc-economy. Carbonation and steel corrosion has been proven to be the main form of damages to the concrete structures durability. Although alkali-activated slag concrete has noticeable excellent properties, previous studies have demonstrated that its carbonation rate is high, which especially be reflected in the low strength grade concrete. Overall,there is little study on its carbonation resistance and there is dispute on its carbonation resistance evaluation, there is no common agreement on the essence of carbonation behavior and the proper technical approach to improve the carbonation resistance of alkali-activated slag concrete has not been established, which is the weak link and is one of the key technologies to restrict its development. Therefore, the investigation of carbonation behaviour and microscopic mechanism of alkali-activated slag cement stone(AASS) would lay a foundation to scientifically evaluate the ability of alkali-activated slag concrete to carbonation resistance and to guide the durability design and the application and development of alkali-activated slag concrete structure.
In this project, alkali-activated slag cement stone(AASS) activated by water glass and NaOH was used to investigate the effect of main factors such as alkali activator type, Na_2O equivalent, water glass module(Ms), water binder ratio(W/B), curing condition and pretreatment method on the carbonation depth and shrinkage behavior. The effect of carbonation on the pH value, Na~+, K~+ and Ca~(2+) content of pore solution of AASS was also studied. The products of carbonation and their microscopic structure were identified by using XRD, SEM, TG-DSC, FT-IR analysis and so on. The effect of carbonation on the pore structure of AASS was analysed by using nitrogen absorption measurement. Based on the technical measures of increasing the alkalinity of solid dispersive phase and reducing the drying shrinkage and soluble alkali content of AASS, technical approach to improve the carbonation resistance of AASS was studed. Chief laws and results are summarized as follows:
In the range of 3%～6%, carbonation depth of AASS decreases with the increase of Na2O equivalent, although the extent of reduction decreases with the increase of Na2O equivalent. At the same Na2O equivalent, the carbonation depth of AASS activated by NaOH is larger than that of AASS activated by water glass. In the range of 1.0～2.0, with the increase of module, carbonation depth of AASS activated by water glass first decreases, then followed by an increase. When Na2O equivalent is 4%~6% and the module of water glass is 1.2~1.5, AASS possesses excellent capability to carbonation resistance. Besides, carbonation depth of AASS increases when W/B increases and decreases when standard curing ages extends. Water curing can increase the carbonation depth of AASS.
Alkali-activated slag cement mortar is more easily carbonated than Portland cement mortars when water-binder ratio is the same. While the consistency of mortars is the same, alkali-activated slag cement mortar used water glass as alkali activator is less carbonated than Portland cement mortar. After being carbonated, the compressive strength of Portland cement mortar increases, while that of alkali-activated slag cement mortar shows the tendency of decline with the increase of carbonation ages within 60 days.
The study on the characteristic of carbonation shrinkage of AASS shows that carbonation doesn’t increase the shrinkage of AASS. In the range of 3%～6%, carbonation shrinkage of AASS decreases with the increase of Na2O equivalent. When water glass is used as the activator, carbonation shrinkage is relatively small with the module of 1.2~1.5. In the range of 0.30～0.35, while W/B increases, carbonation shrinkage of AASS increases and that decreases when standard curing ages extends. Carbonation shrinkage of AASS under water curing is larger than that of standard curing at the same age.
Before carbonation, Na~+ content is more, K~+ content is less, while Ca~(2+) content is much lower in the pore solution of AASS. The pore solution pH value of AASS activated by NaOH is larger than that of AASS activated by water glass. After being 60d carbonated, pH value of pore solution reduces to about 10 and Na~+ content increases, while K~+ and Ca~(2+) content decreases.
When water binder ratio is 0.30, in the AASS activated with water glass, the diameter of main pores is less than 20 nm which volume percentage touches 78%. While in the AASS activated with NaOH, capillary which diameter more than 20nm is more and its volume percentage is 68%. Carbonation increases the amount of the specific surface area of AASS and reduces the average and the most probable distribution pore diameters. C-S-H gel of AASS is an amorphous gel which is more close to tobermorite. C/S ratio of C-S-H gel of AASS activated with water glass is smaller than that of AASS activated with NaOH. Carbonation causes decalcification of C-S-H gel ,so C/S ratio of C-S-H gel decreases, polymerization degree increases. As carbonation products, the main form of CaCO_3 is calcite. With the process of carbonation, vaterite and aragonite come into being. Besides, gaylussite and nahcolite have also been detected. The existence of more alkali (Na~+、K~+) in the pore solution, no existence of Ca(OH)_2 crystal in hydration product and the larger drying shrinkage of alkali- activated slag cement stone are the important reason for its serious carbonation.
Alkali-activated slag cement stone with different activator has its own proper technical approach to improve the carbonation resistance. Increasing the alkalinity of solid dispersive phase is suitable for AASS activated with water glass. Right amount of Ca(OH)_2,Ba(OH)2 and ZnCl_2 can effectively reduce the carbonation depth of AASS. While to AASS activated with NaOH, decrescence of drying shrinkage is useful. Right amount of air entraining agent and Na2SO4 do well to reduce the carbonation depth of AASS.
引文
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