水泥—石灰石粉胶凝体系特性研究
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摘要
为在水泥混凝土中科学、合理和安全地应用石灰石粉,以达到节能利废,同时产生良好的技术、经济和生态效益,本文开展了“水泥-石灰石粉胶凝体系特性研究”,为构建石灰石粉基胶凝材料的制备与应用技术体系提供理论和试验依据。
本文主要工作和取得的研究成果如下:
1.系统研究了C_3S-CaCO_3-H_2O和C_3A-CaCO_3-H_2O两个三元体系的水化特性和相关规律
1)XRD、TG-DSC、IRS微观测试和量热分析表明,CaCO_3促进了C_3S早期水化,阻碍了其后期水化;CaCO_3的加入并未导致C_3S水化产物新相的生成,而主要使C_3S水化历程发生了改变,发现其表现规律为显著压缩了诱导期;25%CaCO_3的掺入使C_3S水化的第一放热峰比纯C_3S的放热峰明显增高、变窄和前移,24h放热量增加18.3%;在系统研究基础上,构建了具有CaCO_3加速特征的C_3S-CaCO_3-H_2O体系水化历程模型。
2)XRD、TG-DSC、IRS分析和SEM观测说明,CaCO_3对C_3A的水化产物C_3AH_6的生成有抑制和加速双重效应,水化初期表现为抑制作用,随着水化的进行,逐渐转为加速作用;CaCO_3抑制了C_4AH_(13)和C_2AH_8的出现,并导致半碳铝酸钙水化物(C_3A·0.5CACO_3·0.5Ca(OH)_2·11.5H_2O)和单碳铝酸钙水化物(C_3A·CaCO_3·11H_2O)的形成;半碳铝酸钙水化物出现在水化初期,水化1d后已全部转变。单碳铝酸钙水化物从水化初期1h至28d一直稳定存在,其形貌特征表现为早期呈长厚片状,随后逐渐向长棒状转变,水化至28d,已转变成细针状;量热分析发现,CaCO_3致使C_3A的水化放热出现了有别于纯C_3A水化放热的“双峰”现象;30%CaCO_3的掺入使24h单位质量C_3A放热量比纯C_3A的放热量增加了2倍多。
2.研究了C_3A-CaSO_4·2H_2O-CaCO_3-H_2O四元体系
由XRD和DSC分析得到,C_3A-CaSO_4·2H_2O-CaCO_3-H_2O四元体系水化产物是C_3AH_6、C3_A·CaCO_3·11H_2O、C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O、AFt和AFm;CaSO_4·2H_2O使C_3AH_6形成时间提前,延迟了单碳铝酸钙和半碳铝酸钙水化物的形成,半碳铝酸钙水化物稳定时间延长;CaCO_3提高了钙矾石的稳定性;通过量热分析,揭示了CaCO_3和CaSO_4·2H_2O共同作用下C_3A水化放热特点,其表现为第一放热峰之后新增加了两个放热峰。
3.研究了工程应用实际体系—水泥-石灰石粉胶凝体系的水化特性及孔结构
1)通过XRD、TG-DSC和量热微观测试分析得出,水泥-石灰石粉胶凝体系水化产物和水化速度与两个三元体系C_3S-CaCO_3-H_2O、C_3A-CaCO_3-H_2O和四元体系C_3A-CaSO_4·2H_2O-CaCO_3-H_2O的规律基本相同。随着石灰石粉掺量增加,单碳铝酸钙形成提前;石灰石粉延迟了钙矾石的生成,对钙矾石起到了稳定作用;石灰石粉改变了水泥水化历程,与纯水泥水化放热相比,10%石灰石粉的掺入致使第一放热峰明显增高、前移,诱导期缩短,提前大约40分钟进入加速期;石灰石粉使单位质量的水泥24h放热量增加了8.5%。
2)MIP分析表明,随水化龄期增长,石灰石粉使水泥浆体孔结构由小孔向大孔转变,产生了孔粗化效应;增大石灰石粉的细度和减小水胶比有利于改善硬化浆体孔结构。
4.研究了水泥-石灰石粉胶凝材料的物理力学性能
1)随石灰石粉掺量增加,浆体流动度减小,砂浆和混凝土的流动度增大,凝结时间缩短;随石灰石粉细度增加,浆体、砂浆和混凝土流动度增大,凝结时间缩短。
2)石灰石粉对水泥早期水化的促进作用,提高了水泥混凝土早期强度,而石灰石粉对水泥混凝土的孔粗化效应导致其后期强度低于基准强度。1d、3d和7d龄期时,随石灰石粉掺量增加,水泥混凝土强度呈先增加后下降的趋势,石灰石粉掺量为10%,增强其早期强度效果最明显,石灰石粉掺量超过20%时,对早期强度没有改善作用。28d龄期时,掺有石灰石粉的水泥混凝土强度全部低于基准强度,石狄石粉掺量愈高,其强度下降愈多。
5.研究了水泥-石灰石粉胶凝体系的耐久性能
1)在硫酸盐以及硫酸盐+氯盐的环境因素下,水泥-石灰石粉胶凝材料耐久性研究表明,其外观破坏形式为试件开裂、表面软化、脱落和溃烂。在单因素(硫酸盐)作用下,6个月时,已造成水化产物碳铝酸钙分解,其破坏主要是由石膏膨胀和碳铝酸钙水化物分解共同造成的;在双因素(硫酸盐+氯盐)作用下,6个月左右时,胶凝材料中主要有CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙过渡产物产生,并有较大量的石膏生成。20个月时,CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙已分解,并产生了易溶于水的CaCl_2。其早期破坏主要因石膏结晶引起体积膨胀造成的,后期破坏主要由石膏以及CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙分解和CaCl_2溶解共同造成并导致腐蚀加剧。
2)无论是在单因素还是在双因素作用下,石灰石粉都加速了水泥基材料的腐蚀破坏,并随石灰石粉掺量增加,其劣化加重。但在双因素作用下,氯盐的存在使试件在腐蚀前后期石膏生成量相差不大,缓解了试件的腐蚀程度。
To achieve scientific,rational and safe use of ground limestone,attain the purpose of energy saving and waste recycling,and consequently bring technical, economic and ecological benefits,the characteristics of cement-ground limestone gelation system is studied in detail in this dissertation.The study results can provide the theoretical and experimental basis for the technical system of production and application of ground limestone based cementitious material.
The main contributions of this thesis are as follows:
1.The hydration characteristic and relative rules of the ternary system of C_3S-CaCO_3-H_2O and C_3A-CaCO_3-H_2O are studied systematically.
1) Microscopic tests of XRD,TG-DSC,IRS and calorimetry show that the addition of CaCO_3 can change the hydration process of C_3S without new hydration product and reduce induction period significantly.The first exothermic peak of the sample containing 25%CaCO_3 appears in advance and is higher and narrower than that of the pure sample.The 24h exothermic quantity increases by 18.3%.Based on these,a hydration process model of C_3S-CaCO_3-H_2O ternary system with acceleration characteristics of CaCO_3 is proposed.
2) XRD,TG-DSC and IRS analysis and SEM observation show that CaCO_3 inhibits the generation of C_3AH_6 at early hydration period but promotes it along with the hydration process.CaCO_3 inhibits the appearance of C_4AH_(13) and C_2AH_8,and causes the formation of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O and C_3A·CaCO_3·11H_2O. The former appears in early hydration,totally being transferred after 1d hydration. The latter exists all the time during the initial hydration to 28d,and their appearance changes from thick flake in early hydration to long rod shape,being fine-needle when hydrated by 28d.The calorimetric analysis indicates that with the addition of CaCO_3. the hydration heat of C_3A has double-peak,which is different from that of pure C_3A only.The hydration heat of C_3A in 24h with the addition of 30%CaCO_3 appears 2 times more than that of the pure C_3A.
2.The hydration characteristic of the quaternary system of C_3A-CaSO_4·2H_2O-CaCO_3-H_2O are studied.
XRD and DSC analysis prove that the hydration products of C_3A-CaSO_4·2H_2O-CaCO_3-H_2O quaternary system are composed of C_3AH_6, C_3A·CaCO_3·11H_2O,C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O,AFt and AFm.The formation time of C_3AH_6 is advanced by CaSO_4·2H_2O.Meanwhile,the hydration products'generation of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O and C_3A·CaCO_3·11H_2O is deferred,and the stability time of hydration product of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O is elongated by CaSO_4·2H_2O.The stability of ettringite is also improved by CaCO_3.The results of calorimetric analysis reveal that the hydration-induced heat-releasing characteristic of C_3A under the co-action of CaCO_3 and CaSO_4·2H_2O is plotted as three peaks.
3.The hydration characteristic and pore structure of cement-ground limestone cementitious material system are studied.
1) XRD,DSC and calorimetric analysis present almost a same law between the cementitious material system and single-mine.With the increase of ground limestone amount,C_3A·CaCO_3·11H_2O advances its generation.Ground limestone defers the formation of ettringite and improves the stability of ettringite.The calorimetric analysis proves that the hydration process of cement is changed by the ground limestone.The addition of 10%ground limestone advances heat-releasing of cement hydration,increases heat-releasing speed and amount,shortens the induction period, advances the entering into the acceleration period ahead about 40 minutes and increases 8.5%heat of cement of per unit mass in 24h.
2) The amount and fineness of ground limestone and water-binder ratio have effect on pore structure of harden paste by MIP analysis.The more the limestone is, the bigger the average diameter of harmful pore is,which means ground limestone increasing the probability of internal defect in cement paste.Using finer ground limestone and reducing water-binder ratio are beneficial to improve the pore structure of harden paste.
4.The physical and mechanical property of cement-ground limestone cementitious material system are studied.
1) With the increase of ground limestone amount,the fluidity of paste reduces while the fluidity of mortar and concrete increases,and the setting time is shortened. With the increases of ground limestone fineness,the fluidity of paste,mortar or concrete increases and the setting time is shortened.
2) Ground limestone promotes the earlier hydration of cement and early strength of cement and concrete,but makes the later strength lower than normal concrete due to its pore coarsening effect.The strength of cement and concrete at 1d,3d and 7d increase firstly and then decrease along with the increasing of ground limestone.10% of ground limestone has the most obvious effect on improving early strength.When the amount of ground limestone is more than 20%,the addition of ground limestone does not improve the early strength(1～7d) of concrete.The strength of the sample containing ground limestone at 28d is lower than normal concrete,and the more of the limestone,the lower of the strength.
5.The durability of cement-ground limestone cementitious material system are studied.
1) Under the condition of sulfate or sulfate and chloride,the study on the durability of cement-ground limestone cementitious materials shows that the damages of the appearance including cracking,softening,abscission and ulceration.Under the action of single factor(sulfate),the hydration product of calcium carboaluminate can be decomposed after 6 months.The damage of specimens is mainly induced by the expansion of gypsum and the decomposition of hydration products of calcium carboaluminate.Under the action of two factors(sulfate+chloride),CaAl_2 (CO_3)_2(OH)_4·6H_2O and transition product of calcium chloroaluminate are produced in the cementitious materials,accompanying with the appearance of much gypsum after 6 months.Both CaAl_2(CO_3)_2(OH)_4·6H_2O and calcium chloroaluminate can be decomposed,producing easy-soluble CaCl_2 after 20 months.Early damage of specimens is caused by volume expansion induced by gypsum crystallization,while further damage is mainly caused by gypsum,decomposition of CaAl_2(CO_3)_2(OH)_4·6H_2O and calcium chloroaluminate,and the dissolution of CaCl_2.
2) The ground limestone accelerate the erosion damage of cement-based materials regardless of single factor or two factors,and the more of the ground limestone,the more of the deterioration.But under the two factors,chloride ions make no obvious difference in the generation of gypsum for the sample before and after being eroded,which relieves the erosion degree of the sample.
本文主要工作和取得的研究成果如下:
1.系统研究了C_3S-CaCO_3-H_2O和C_3A-CaCO_3-H_2O两个三元体系的水化特性和相关规律
1)XRD、TG-DSC、IRS微观测试和量热分析表明,CaCO_3促进了C_3S早期水化,阻碍了其后期水化;CaCO_3的加入并未导致C_3S水化产物新相的生成,而主要使C_3S水化历程发生了改变,发现其表现规律为显著压缩了诱导期;25%CaCO_3的掺入使C_3S水化的第一放热峰比纯C_3S的放热峰明显增高、变窄和前移,24h放热量增加18.3%;在系统研究基础上,构建了具有CaCO_3加速特征的C_3S-CaCO_3-H_2O体系水化历程模型。
2)XRD、TG-DSC、IRS分析和SEM观测说明,CaCO_3对C_3A的水化产物C_3AH_6的生成有抑制和加速双重效应,水化初期表现为抑制作用,随着水化的进行,逐渐转为加速作用;CaCO_3抑制了C_4AH_(13)和C_2AH_8的出现,并导致半碳铝酸钙水化物(C_3A·0.5CACO_3·0.5Ca(OH)_2·11.5H_2O)和单碳铝酸钙水化物(C_3A·CaCO_3·11H_2O)的形成;半碳铝酸钙水化物出现在水化初期,水化1d后已全部转变。单碳铝酸钙水化物从水化初期1h至28d一直稳定存在,其形貌特征表现为早期呈长厚片状,随后逐渐向长棒状转变,水化至28d,已转变成细针状;量热分析发现,CaCO_3致使C_3A的水化放热出现了有别于纯C_3A水化放热的“双峰”现象;30%CaCO_3的掺入使24h单位质量C_3A放热量比纯C_3A的放热量增加了2倍多。
2.研究了C_3A-CaSO_4·2H_2O-CaCO_3-H_2O四元体系
由XRD和DSC分析得到,C_3A-CaSO_4·2H_2O-CaCO_3-H_2O四元体系水化产物是C_3AH_6、C3_A·CaCO_3·11H_2O、C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O、AFt和AFm;CaSO_4·2H_2O使C_3AH_6形成时间提前,延迟了单碳铝酸钙和半碳铝酸钙水化物的形成,半碳铝酸钙水化物稳定时间延长;CaCO_3提高了钙矾石的稳定性;通过量热分析,揭示了CaCO_3和CaSO_4·2H_2O共同作用下C_3A水化放热特点,其表现为第一放热峰之后新增加了两个放热峰。
3.研究了工程应用实际体系—水泥-石灰石粉胶凝体系的水化特性及孔结构
1)通过XRD、TG-DSC和量热微观测试分析得出,水泥-石灰石粉胶凝体系水化产物和水化速度与两个三元体系C_3S-CaCO_3-H_2O、C_3A-CaCO_3-H_2O和四元体系C_3A-CaSO_4·2H_2O-CaCO_3-H_2O的规律基本相同。随着石灰石粉掺量增加,单碳铝酸钙形成提前;石灰石粉延迟了钙矾石的生成,对钙矾石起到了稳定作用;石灰石粉改变了水泥水化历程,与纯水泥水化放热相比,10%石灰石粉的掺入致使第一放热峰明显增高、前移,诱导期缩短,提前大约40分钟进入加速期;石灰石粉使单位质量的水泥24h放热量增加了8.5%。
2)MIP分析表明,随水化龄期增长,石灰石粉使水泥浆体孔结构由小孔向大孔转变,产生了孔粗化效应;增大石灰石粉的细度和减小水胶比有利于改善硬化浆体孔结构。
4.研究了水泥-石灰石粉胶凝材料的物理力学性能
1)随石灰石粉掺量增加,浆体流动度减小,砂浆和混凝土的流动度增大,凝结时间缩短;随石灰石粉细度增加,浆体、砂浆和混凝土流动度增大,凝结时间缩短。
2)石灰石粉对水泥早期水化的促进作用,提高了水泥混凝土早期强度,而石灰石粉对水泥混凝土的孔粗化效应导致其后期强度低于基准强度。1d、3d和7d龄期时,随石灰石粉掺量增加,水泥混凝土强度呈先增加后下降的趋势,石灰石粉掺量为10%,增强其早期强度效果最明显,石灰石粉掺量超过20%时,对早期强度没有改善作用。28d龄期时,掺有石灰石粉的水泥混凝土强度全部低于基准强度,石狄石粉掺量愈高,其强度下降愈多。
5.研究了水泥-石灰石粉胶凝体系的耐久性能
1)在硫酸盐以及硫酸盐+氯盐的环境因素下,水泥-石灰石粉胶凝材料耐久性研究表明,其外观破坏形式为试件开裂、表面软化、脱落和溃烂。在单因素(硫酸盐)作用下,6个月时,已造成水化产物碳铝酸钙分解,其破坏主要是由石膏膨胀和碳铝酸钙水化物分解共同造成的;在双因素(硫酸盐+氯盐)作用下,6个月左右时,胶凝材料中主要有CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙过渡产物产生,并有较大量的石膏生成。20个月时,CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙已分解,并产生了易溶于水的CaCl_2。其早期破坏主要因石膏结晶引起体积膨胀造成的,后期破坏主要由石膏以及CaAl_2(CO_3)_2(OH)_4·6H_2O和氯铝酸钙分解和CaCl_2溶解共同造成并导致腐蚀加剧。
2)无论是在单因素还是在双因素作用下,石灰石粉都加速了水泥基材料的腐蚀破坏,并随石灰石粉掺量增加,其劣化加重。但在双因素作用下,氯盐的存在使试件在腐蚀前后期石膏生成量相差不大,缓解了试件的腐蚀程度。
To achieve scientific,rational and safe use of ground limestone,attain the purpose of energy saving and waste recycling,and consequently bring technical, economic and ecological benefits,the characteristics of cement-ground limestone gelation system is studied in detail in this dissertation.The study results can provide the theoretical and experimental basis for the technical system of production and application of ground limestone based cementitious material.
The main contributions of this thesis are as follows:
1.The hydration characteristic and relative rules of the ternary system of C_3S-CaCO_3-H_2O and C_3A-CaCO_3-H_2O are studied systematically.
1) Microscopic tests of XRD,TG-DSC,IRS and calorimetry show that the addition of CaCO_3 can change the hydration process of C_3S without new hydration product and reduce induction period significantly.The first exothermic peak of the sample containing 25%CaCO_3 appears in advance and is higher and narrower than that of the pure sample.The 24h exothermic quantity increases by 18.3%.Based on these,a hydration process model of C_3S-CaCO_3-H_2O ternary system with acceleration characteristics of CaCO_3 is proposed.
2) XRD,TG-DSC and IRS analysis and SEM observation show that CaCO_3 inhibits the generation of C_3AH_6 at early hydration period but promotes it along with the hydration process.CaCO_3 inhibits the appearance of C_4AH_(13) and C_2AH_8,and causes the formation of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O and C_3A·CaCO_3·11H_2O. The former appears in early hydration,totally being transferred after 1d hydration. The latter exists all the time during the initial hydration to 28d,and their appearance changes from thick flake in early hydration to long rod shape,being fine-needle when hydrated by 28d.The calorimetric analysis indicates that with the addition of CaCO_3. the hydration heat of C_3A has double-peak,which is different from that of pure C_3A only.The hydration heat of C_3A in 24h with the addition of 30%CaCO_3 appears 2 times more than that of the pure C_3A.
2.The hydration characteristic of the quaternary system of C_3A-CaSO_4·2H_2O-CaCO_3-H_2O are studied.
XRD and DSC analysis prove that the hydration products of C_3A-CaSO_4·2H_2O-CaCO_3-H_2O quaternary system are composed of C_3AH_6, C_3A·CaCO_3·11H_2O,C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O,AFt and AFm.The formation time of C_3AH_6 is advanced by CaSO_4·2H_2O.Meanwhile,the hydration products'generation of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O and C_3A·CaCO_3·11H_2O is deferred,and the stability time of hydration product of C_3A·0.5CaCO_3·0.5Ca(OH)_2·11.5H_2O is elongated by CaSO_4·2H_2O.The stability of ettringite is also improved by CaCO_3.The results of calorimetric analysis reveal that the hydration-induced heat-releasing characteristic of C_3A under the co-action of CaCO_3 and CaSO_4·2H_2O is plotted as three peaks.
3.The hydration characteristic and pore structure of cement-ground limestone cementitious material system are studied.
1) XRD,DSC and calorimetric analysis present almost a same law between the cementitious material system and single-mine.With the increase of ground limestone amount,C_3A·CaCO_3·11H_2O advances its generation.Ground limestone defers the formation of ettringite and improves the stability of ettringite.The calorimetric analysis proves that the hydration process of cement is changed by the ground limestone.The addition of 10%ground limestone advances heat-releasing of cement hydration,increases heat-releasing speed and amount,shortens the induction period, advances the entering into the acceleration period ahead about 40 minutes and increases 8.5%heat of cement of per unit mass in 24h.
2) The amount and fineness of ground limestone and water-binder ratio have effect on pore structure of harden paste by MIP analysis.The more the limestone is, the bigger the average diameter of harmful pore is,which means ground limestone increasing the probability of internal defect in cement paste.Using finer ground limestone and reducing water-binder ratio are beneficial to improve the pore structure of harden paste.
4.The physical and mechanical property of cement-ground limestone cementitious material system are studied.
1) With the increase of ground limestone amount,the fluidity of paste reduces while the fluidity of mortar and concrete increases,and the setting time is shortened. With the increases of ground limestone fineness,the fluidity of paste,mortar or concrete increases and the setting time is shortened.
2) Ground limestone promotes the earlier hydration of cement and early strength of cement and concrete,but makes the later strength lower than normal concrete due to its pore coarsening effect.The strength of cement and concrete at 1d,3d and 7d increase firstly and then decrease along with the increasing of ground limestone.10% of ground limestone has the most obvious effect on improving early strength.When the amount of ground limestone is more than 20%,the addition of ground limestone does not improve the early strength(1～7d) of concrete.The strength of the sample containing ground limestone at 28d is lower than normal concrete,and the more of the limestone,the lower of the strength.
5.The durability of cement-ground limestone cementitious material system are studied.
1) Under the condition of sulfate or sulfate and chloride,the study on the durability of cement-ground limestone cementitious materials shows that the damages of the appearance including cracking,softening,abscission and ulceration.Under the action of single factor(sulfate),the hydration product of calcium carboaluminate can be decomposed after 6 months.The damage of specimens is mainly induced by the expansion of gypsum and the decomposition of hydration products of calcium carboaluminate.Under the action of two factors(sulfate+chloride),CaAl_2 (CO_3)_2(OH)_4·6H_2O and transition product of calcium chloroaluminate are produced in the cementitious materials,accompanying with the appearance of much gypsum after 6 months.Both CaAl_2(CO_3)_2(OH)_4·6H_2O and calcium chloroaluminate can be decomposed,producing easy-soluble CaCl_2 after 20 months.Early damage of specimens is caused by volume expansion induced by gypsum crystallization,while further damage is mainly caused by gypsum,decomposition of CaAl_2(CO_3)_2(OH)_4·6H_2O and calcium chloroaluminate,and the dissolution of CaCl_2.
2) The ground limestone accelerate the erosion damage of cement-based materials regardless of single factor or two factors,and the more of the ground limestone,the more of the deterioration.But under the two factors,chloride ions make no obvious difference in the generation of gypsum for the sample before and after being eroded,which relieves the erosion degree of the sample.
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