Effect of mineral microcapsules on self-healing properties of cement mortar
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摘要: 水泥基复合材料受多种物化因素的影响易开裂，从而影响其耐久性能。提升水泥基复合材料的裂缝自修复性能，是提高其耐久性和降低整个生命周期维护成本的关键。因此，基于结晶膨胀、储水释水、助剂补强三种功能特性，本文以复合膨胀剂、Na-膨润土和滑石粉三种矿物为芯材，碱激发材料(水玻璃激发偏高岭土)为壁材，研发了一种集修复补强一体的全无机微胶囊型水泥基裂缝自修复材料。基于本征力学性能研究，以强度恢复率、裂缝宽度愈合率、裂缝面积修复率为评价指标，探究了微胶囊对水泥砂浆试件裂缝自修复效果的影响规律，通过微观测试分析了修复机理。结果表明，随着微胶囊掺量的增加，砂浆强度呈现先增加后减小的趋势；当其掺量为10%时，砂浆28d抗折和抗压强度最高，较空白组分别提高了6.17%和4.39%。同掺量下，二次养护28d强度恢复率达到了115.5%，35d时30条裂缝的平均面积修复率和归一化裂缝面积修复率分别为100%和72.3%，远高于空白组的55.3%和37.7%。XRD和SEM分析表明，二次养护条件下裂缝处生成了大量的Ca(OH)2、AFt、CaCO3、Mg3Ca(CO3)4以及C-S-H凝胶等微膨胀、高强、胶凝性好的水化产物，从而实现快速填充、修复裂缝和补强。Abstract: Cement-based composites are prone to cracking under the influence of many physical and chemical factors, which affects their durability. Improving the crack self-healing performance of cement-based composites is the key to improve their durability and reduce the maintenance cost throughout their life cycle. Therefore, based on the three functional characteristics of crystal expansion, water storage and release, and auxiliary reinforcement, this paper developed an all-inorganic microcapsule cement-based crack self-healing material integrating repair and reinforcement, with three minerals, namely composite expansion agent, Na-bentonite and talc powder, as the core material, and alkali exciting material (water glass stimulated metakaolin) as the wall material. Based on the study of intrinsic mechanical properties, with strength recovery rate, crack width healing rate and crack area healing rate as evaluation indexes, the influence of microcapsule on the crack self-healing effect of cement mortar specimens was explored, and the self-healing mechanisms were analyzed through microscopic testing. The results show that the strength of mortar increases first and then decreases with the increase of microcapsule content. When the dosage is 10%, the 28d flexural and compressive strengths of mortar are the highest, which are 6.17% and 4.39% higher than that of blank group, respectively. With the same dosage, the strength recovery rate reaches 115.5% after secondary cured in water for 28 days, and both the average and normalized crack area healing rates are 100% and 72.3%, respectively, at 35d, which are much higher than 55.3% and 37.7% of the blank group. The XRD and SEM analysis show that under the condition of secondary curing, a large number of hydration products such as Ca(OH)2, AFt, CaCO3, Mg3Ca(CO3)4 and C-S-H gel with micro-expansion, high strength and good cementitious properties are generated at the crack, so as to realize rapid filling, repairing and reinforcing of cracks.
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图 5 浸泡后微胶囊吸水率随时间的变化
Figure 5. Changes of water absorption of microcapsules with time after immersion
图 6 微胶囊掺量对砂浆试件抗折强度和抗压强度的影响
Figure 6. Influence of microcapsule content on flexural strength and compressive strength of mortar specimens
图 7 不同微胶囊掺量的砂浆试件的强度恢复率和提升百分数
Figure 7. Strength recovery rate and strength recovery improvement rate with microcapsule dosage
图 8 不同微胶囊掺量的砂浆试件裂缝愈合效果随龄期变化的直观图
Figure 8. Direct view of the change about crack healing effect of mortar specimens of different microcapsule dosage with age
图 9 不同龄期不同裂缝宽度的裂缝宽度愈合率
Figure 9. Crack width healing rate at different ages and different crack widths
图 10 砂浆试件裂缝愈合效果随龄期和微胶囊掺量的变化的黑白图
Figure 10. Black and white chart of the changes about crack healing effect of mortar specimens with microcapsule dosage and age
图 11 平均裂缝面积修复率和提升百分数在不同微胶囊掺量下随龄期的变化
Figure 11. Change of average crack area healing rate and crack area healing improvement rate with age under different microcapsule dosage
图 12 不同掺量不同龄期的微胶囊试件的归一化裂缝面积修复率
Figure 12. Normalized crack area healing rate of microcapsule specimens with different dosage and different ages
图 13 砂浆裂缝自修复效果在不同环境因素下的分析：(a) 雷达图；(b) 封闭区域面积
Figure 13. Analysis of self-healing effect of mortar cracks under different environmental factors: (a) Radar map; (b) Enclosed areas
图 14 空白组和微胶囊掺量10%的砂浆试件裂缝处生成物的XRD图谱
Figure 14. XRD pattern of the product at the crack of blank group and mortar test group with 10% microcapsule content
图 15 微胶囊掺量10%的胶砂试件裂缝处生成物的SEM图像和EDS图谱
(图(a) ①、②的EDS对应图(c) ①、②，图(b) ③、④的EDS图对应图(d) ③、④)
Figure 15. SEM photos and EDS spectrum of the product at the crack of the mortar sample with 10% microcapsule content
(The EDS in Figure (a) ① and ② correspond to the EDS in Figure (c) ① and ②, and the EDS in Figure (b) ③、④ correspond to the EDS in Figure (d) ③、④)
图 16 掺微胶囊砂浆的裂缝修复过程示意图
Figure 16. Schematic illustration of crack healing process of microencapsulated mortar
表 1 各原材料的化学组成(wt%)
Table 1. Chemical composition of each raw material (wt%)
Material CaO SiO2 Al2O3 Fe2O3 MgO SO3 K2O Na2O TiO2 Loss Cement 61.56 20.56 5.65 3.45 2.36 2.26 0.75 0.18 — 2.22 Metakaolin 0.38 55.50 40.90 0.56 0.21 — 0.24 0.35 1.34 — Compound expansion agent 69.90 2.74 1.62 0.68 2.63 21.60 0.33 0.11 0.12 — Talc powder 3.60 42.30 — 0.27 53.60 — — — — — Na-Bentonite 5.91 73.00 12.00 0.89 3.62 — 2.44 1.85 0.10 — 
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表 2 膨胀剂性能指标
Table 2. Performance index of expansion agent
Test item Standard value Test value Fineness Specific surface area/(m2·kg−1) ≥200 235 Setting time Initial setting/(hour: minute) ≥0:45 1:35 Final setting/(hour: min) ≤6:00 2:52 Limited expansion rate 7 d in water/% ≥0.035 0.156 Compressive strength 7 d/MPa ≥22.5 23.6
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表 3 测试力学性能的砂浆试件原材料配比
Table 3. Raw material ratio of mortar specimens for testing mechanical properties
Microcapsule content/% Sand/g Cement/g Water/g Self-healing material/g 0 1350 450 225 0 5 1282.5 450 225 67.5 10 1215 450 225 135 15 1 012.5 450 225 202.5
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表 4 需要压制裂缝的砂浆试件原材料配比
Table 4. Raw material ratio of mortar specimen to suppress cracks
Microcapsule content/% Sand/g Cement/g Water/g Self-healing material/g Polypropylene fibre/g 0 1350 450 225 0 2.25 5 1282.5 450 225 67.5 2.25 10 1215 450 225 135 2.25 15 1012.5 450 225 202.5 2.25
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