粘土固化型微胶囊复合水泥基材料的设计与力学损伤自修复行为

马衍轩; 吴睿; 葛亚杰; 黄昊; 付双阳; 张建

doi:10.13801/j.cnki.fhclxb.20230112.002

粘土固化型微胶囊复合水泥基材料的设计与力学损伤自修复行为

doi: 10.13801/j.cnki.fhclxb.20230112.002

马衍轩^{1, 2, 3, ,},
吴睿^1,,
葛亚杰¹,
黄昊³,
付双阳¹,
张建⁴

1.
青岛理工大学　土木工程学院，青岛 266520
2.
海洋环境混凝土技术教育部工程研究中心，青岛 266520
3.
中国水利水电科学研究院流域水循环模拟与调控国家重点实验室，北京 100038
4.
青岛青新阳光集团有限公司，青岛 266404

基金项目: 山东省自然科学基金项目(ZR2022 ME121)；青岛西海岸新区2020 年科技计划专项项目(2020-38)；海洋环境混凝土技术教育部工程研究中心开放课题(TMduracon2022010)；中国水利水电科学研究院流域水循环模拟与调控国家重点实验室开放研究基金项目(IWHR-SKL-202106)；国家自然科学基金(51408330)

详细信息

通讯作者:
马衍轩，博士，副教授，硕士生导师，研究方向为防灾减灾建筑材料与技术　E-mail: yxma@qut.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2022-10-19
- 修回日期: 2022-12-09
- 录用日期: 2023-01-01
- 网络出版日期: 2023-01-12
- 刊出日期: 2023-09-15

Design and self-repair behavior of clay-cured microcapsule composite cementitious materials

MA Yanxuan^{1, 2, 3
, ,},
WU Rui^1
,,
GE Yajie¹,
HUANG Hao³,
FU Shuangyang¹,
ZHANG Jian⁴

1.
School of Civil Engineering, Qingdao University of Technology, Qingdao 266520, China
2.
Engineering Research Center of Concrete Technology under Marine Environment, Ministry of Education, Qingdao 266520, China
3.
State Key Laboratory of Simulation and Regulation of Water Cycle in River Basin, China Institute of Water Resources and Hydropower Research, Beijing 100038, China
4.
Qingdao Qingxin Sunshine Group CO., LTD., Qingdao 266404, China

Funds: Shandong Provincial Natural Science Foundation (ZR2022 ME121); Special Project of Science and Technology Plan in 2020 of Qingdao West Coast New Area, China (2020-38); Open Research Fund of Engineering Research Center of Concrete Technology under Marine Environment, Ministry of Education (TMduracon2022010); Open Research Fund of State Key Laboratory of Simulation and Regulation of Water Cycle in River Basin (China Institute of Water Resources and Hydropower Research) (IWHR-SKL-202106); National Natural Science Foundation of China Project (51408330)

摘要

摘要: 采用圆锅造粒法，通过对微胶囊工艺与配方参数进行设计和优化，制备了以粘土固化剂、膨润土、MgO膨胀剂和微晶纤维素为芯材，以乙基纤维素(EC)为壁材的微胶囊，采用正交试验探索了微胶囊芯材组分对自修复微胶囊/水泥基复合材料自修复效果的影响并确定了微胶囊芯材的最佳组成为：粘土固化剂为10wt%、MgO膨胀剂为35wt%、微晶纤维素为6wt%，膨润土为49wt%。研究结果表明，随着微胶囊掺量的增加，自修复水泥基材料的抗压强度降低，当微胶囊掺量(占水泥质量)为3%时，自修复微胶囊/水泥基复合材料的抗压强度相较于空白组仅下降了4%且具有较高的强度恢复率为103.8%。通过数字散斑相关方法(DSCM)对加载过程中的自修复微胶囊/水泥基复合材料的变形行为进行了追踪测试。从应力-应变曲线、应变场分布、灰度相关系数特征值(S_tc)和应变特征值(S_ts)之间的变化规律，得出自修复微胶囊/水泥基复合材料的自修复机制，基于微胶囊破裂时产生了与水泥基同源物质钙钒石(AFt)和Mg(OH)₂对裂纹进行填补，限制裂纹发展，达到修复裂纹的目的。
- 微胶囊 /
- 水泥基材料 /
- 粘土固化 /
- 力学损伤 /
- 自修复行为
Abstract: Using the round pot granulation method, through the design and optimization of the microcapsule process and formulation parameters, microcapsules with clay solidifying agent, bentonite, MgO expansion agent and microcrystalline cellulose as the core material and ethyl cellulose (EC) as the core material were prepared. For the microcapsules of the wall material, the influence of the components of the microcapsule core material on the self-healing effect of the self-healing microcapsule/cementitious composite material was explored by orthogonal experiments, and the optimal composition of the microcapsule core material was determined: That is, the clay curing agent is 10wt% , MgO expansion agent is 35wt%, microcrystalline cellulose is 6wt%, and bentonite is 49wt%. The results show that the compressive strength of self-healing microcapsule/cementitious composite decreases with the increase of the content of microcapsules. When the content (mass to cement) of microcapsules is 3%, the compressive strength of self-healing microcapsule/cementitious composite is only dropped by 4% with a high strength recovery rate of 103.8%. The deformation behavior of self-healing microcapsule/cementitious composites during loading was traced and tested by the digital speckle correlation method (DSCM). From the stress-strain curve, strain field distribution, gray correlation coefficient eigenvalues (S_tc) and strain eigenvalues (S_ts), the self-healing mechanism of self-healing microcapsule/cementitious composite is based on the fact that when the microcapsules rupture, the cement-based homologous substances (AFt, Mg(OH)₂) are generated to fill the cracks, limit the development of cracks, and achieve the purpose of repairing cracks.
- microcapsule /
- cement-based material /
- clay curing /
- mechanical damage /
- self-healing behavior

HTML全文

图 1 微胶囊修复机制示意图

Figure 1. Diagram of microcapsule repair mechanis

AFt—Calciovanadite

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图 2 不同转速下粒径为0.1~1.0 mm的微胶囊的产率分布

Figure 2. Yield distribution of particle size from 0.1-1.0 mm microcapsules at different rotational speeds

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图 3 不同乙基纤维素(EC)溶液掺量下粒径为0.1~1.0 mm的微胶囊的产率分布

Figure 3. Yield distribution of particle size from 0.1-1.0 mm microcapsules under different ethyl cellulose (EC) solution contents

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图 4 不同EC溶液浓度下粒径为0.1~1.0 mm的微胶囊的产率分布

Figure 4. Yield distribution of particle size from 0.1-1.0 mm microcapsules under different EC solution concentrations

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图 5 纯EC和微胶囊的FTIR图谱

Figure 5. FTIR spectra of EC and microcapsules

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图 6 0.1~0.2 mm范围内微胶囊的粒径分布 (a)、长径比 (b) 和圆形度 (c)

Figure 6. Particle size distribution (a), aspect ratio (b) and circularity (c) of microcapsules in the range of 0.1-0.2 mm

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图 7 微胶囊的微观形貌

Figure 7. Micro-morphology of microcapsules

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图 8 不同掺量微胶囊/水泥基复合材料断面微观形貌：((a₁), (a₂)) 0%；((b₁), (b₂)) 3%

Figure 8. Micro-morphologies of cross-sections of microcapsules/cementitious composites with different dosages: ((a₁), (a₂)) 0%; ((b₁), (b₂)) 3%

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图 9 微胶囊、水泥基体和微胶囊/水泥基复合材料的XRD图谱

Figure 9. XRD patterns of microcapsules, cementitious substrates and microcapsules/cementitious composites

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图 10 微胶囊/水泥基复合材料的化学组成

Figure 10. Chemical composition of the microcapsule/cementitious composites

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图 11 不同掺量的微胶囊在水泥基体中的分散状态：(a) 0%；(b) 3%；(c) 6%；(d) 9%

Figure 11. Dispersion state of different microcapsule dosages in cement matrix: (a) 0%; (b) 3%; (c) 6%; (d) 9%

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图 12 不同微胶囊掺量的自修复水泥基复合材料的抗压强度

Figure 12. Compressive strength of self-healing cement-based composites with different microcapsule contents

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图 13 微胶囊/水泥基复合材料的强度恢复率

Figure 13. Strength recovery rate of microcapsule/cementitious composites

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图 14 空白组样品修复后的应力-应变、灰度相关系数特征值S_tc和X 方向应变特征值S_ts的关系曲线

Figure 14. Relationship curves of stress-strain, gray correlation coefficient characteristic value S_tc and Characteristic value of strain in X direction S_ts of blank group samples after repair

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图 15 不同微胶囊掺量的水泥基自修复材料样品预压至60%极限抗弯应力(σ_max)(左)和在大气环境下修复后加载至60% σ_max(右)X方向的应变场：((a), (b)) 0%；((c), (d)) 3%

Figure 15. Samples of cement-based self-repairing materials with different content of microcapsules were pre-pressed to 60% σ_max (left) and the strain field loaded to 60% maximum bending stress (σ_max)(right) X direction after repair in atmospheric environment: ((a), (b)) 0%; ((c), (d)) 3%

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图 16 含3%微胶囊的水泥基自修复材料样品修复后的应力-应变、S_tc和S_ts的关系曲线

Figure 16. Relationship curves of stress-strain, S_tc and S_ts of cement-based self-healing materials containing 3% microcapsules after repair

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表 1 微胶囊固料配合比

Table 1. Solid material mix ratio of microcapsules

Clay curing agent/wt%	MgO expansion agent/wt%	Microcrystalline cellulose/wt%	Bentonite/ wt%
10	35	6	49

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表 2 微胶囊组分三因素四水平正交试验设计表

Table 2. Three-factors and four-levels orthogonal experimental design of microcapsule components

No.	A	B	C	D
No.	Clay curing agent/wt%	MgO expansion agent/wt%	Microcrystalline cellulose/wt%	Bentonite/wt%
1(A₁B₁C₁)	5	5	2	88
2(A₁B₂C₂)	5	15	4	76
3(A₁B₃C₃)	5	25	6	64
4(A₁B₄C₄)	5	35	8	52
5(A₂B₁C₂)	10	5	4	81
6(A₂B₂C₁)	10	15	2	73
7(A₂B₃C₄)	10	25	8	57
8(A₂B₄C₃)	10	35	6	49
9(A₃B₁C₃)	15	5	6	74
10(A₃B₂C₄)	15	15	8	62
11(A₃B₃C₁)	15	25	2	58
12(A₃B₄C₂)	15	35	4	46
13(A₄B₁C₄)	20	5	8	67
14(A₄B₂C₃)	20	15	6	59
15(A₄B₃C₂)	20	25	4	51
16(A₄B₄C₁)	20	35	2	43

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表 3 微胶囊囊芯组分对自修复微胶囊/水泥基复合材料的抗压强度和强度恢复率的影响正交试验结果

Table 3. Effects of microcapsule core components on compressive strength and strength recovery rate of self-healing microcapsule/cement-based composites: Orthogonal test results

No.	Compressive strength /MPa	Repair strength /MPa	Repair efficiency /%
1(A₁B₁C₁)	52.2	58.7	112.5
2(A₁B₂C₂)	45.4	56.3	124.0
3(A₁B₃C₃)	52.6	58.6	111.4
4(A₁B₄C₄)	61.4	77.6	121.1
5(A₂B₁C₂)	73.4	76.8	104.7
6(A₂B₂C₁)	68.3	57.7	84.4
7(A₂B₃C₄)	55.6	73.3	131.9
8(A₂B₄C₃)	76.4	79.3	103.8
9(A₃B₁C₃)	62.2	73.5	118.2
10(A₃B₂C₄)	69.3	62.5	90.2
11(A₃B₃C₁)	67.2	67.0	99.7
12(A₃B₄C₂)	59.4	34.3	57.7
13(A₄B₁C₄)	62.9	57.1	90.8
14(A₄B₂C₃)	68.6	56.0	81.6
15(A₄B₃C₂)	72.7	64.5	88.7
16(A₄B₄C₁)	68.2	70.0	102.6

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表 4 以水泥基自修复材料抗压强度为指标的方差统计F值分析表

Table 4. Statistics of variance F value analysis table with compressive strength of cement-based self-repairing materials as index

Factor	Sums of squared deviations	Degree of freedom	Mean square	F
A	635.30	3	211.77	5.17
B	45.35	3	15.12	0.17
C	17.47	3	5.82	0.06

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表 5 各因素对水泥基自修复材料抗压强度作用的均值分析表

Table 5. Analysis of the mean value of each factor against compressive strength

Factor	K_1j	K_2j	K_3j	K_4j
A	52.900	68.425	64.525	68.100
B	62.675	62.900	62.025	66.350
C	63.975	62.725	64.950	62.300
Note: K_ij—The ith average value of factor j.

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表 6 以水泥基自修复材料修复效率为指标的F值分析表

Table 6. F value analysis table with repair efficiency of cement-based self-repairing materials as index

Factor	Sums of squared deviations	Degree of freedom	Mean square	F
A	1931.91	3	643.97	2.26
B	541.60	3	180.56	0.45
C	466.48	3	155.49	0.38

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表 7 各因素对水泥基自修复材料修复效率作用的均值分析表

Table 7. Analysis of means table of the effects of various factors on the repair efficiency of cement-based self-repairing materials

Factor	K_1j	K_2j	K_3j	K_4j
A	117.250	106.200	91.450	90.925
B	106.550	95.050	107.925	97.425
C	99.800	93.775	103.750	108.500

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