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摘要: 為探究干濕循環對水泥基復合充填材料長期穩定性的影響，以水灰比4∶1水泥基復合材料為研究對象，借助ETM力學試驗系統、X射線衍射及掃描電鏡掃描裝置，對不同干濕循環次數下“飽水”狀態和“失水”狀態的試件進行單軸抗壓強度試驗，并通過物相分析及微觀結構探討干濕循環對其影響機理。結果表明，隨著干濕循環次數的增加，“飽水”狀態下失水率逐漸增大，含水率和容重呈下降趨勢，峰值強度先增加后減小，增幅最高達9%；“失水”狀態下失水率、含水率和容重均變化不大，峰值強度較初始狀態有所降低，最高達13.5%；兩種狀態彈性模量和殘余強度都呈下降趨勢。通過機理分析發現，“干”過程中碳化反應是材料強度降低的主要原因，而“濕”過程中吸水將部分碳酸鈣等物質轉化為具有承載能力的鈣礬石（AFT）和碳硫硅鈣石（TSA）是材料強度恢復的主要原因，但恢復能力有限，長期的干濕循環會對水泥基復合充填材料穩定性產生不利影響。Abstract: In recent years, cement-based composite materials have been widely used in mine filling, which can well solve the hidden danger of goaf collapse. However, when the water table and surrounding rock moisture content change, the filling materials will be in the process of dry and wet alternation, which will affect the long-term stability of the filling materials and goaf. In order to explore the influence of dry and wet cycles on the long-term stability of cement-based composite filling materials, taking water-cement ratio 4∶1 cement-based composites as the research object and using ETM mechanical test system, X-ray diffraction (XRD) and scanning electron microscopy (SEM) device, uniaxial compressive strength tests were carried out in the state of "water saturation" and "water loss" under different dry-wet circulation. The influence mechanism of dry-wet circulation was discussed by phase analysis and microstructure. The results show that as the number of dry-wet circulation increases, the loss rate increases gradually while the water content and bulk density decrease, the peak intensity first increases and then decreases, and the increase is as high as 9% under the saturated state. The water loss rate, water content and bulk density do not change much under the condition of "water loss", while the peak strength decreases from the initial state to up to 13.5%. The elastic modulus and residual strength of the two states show a downward trend. Through mechanism analysis, it is found that carbonation reaction is the main reason for material strength reduction in the "dry" process, while the CaCO3 and other materials are converted into ettringite (AFT) and thaumasite (TSA) with some bearing capacity during the absorbing water process in "wet" process, which is the main reason for the strength recovery of materials. However, the recovery ability is limited, and the long-term dry-wet circulation will adversely affect the stability of cement-based composite filling material.
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Key words:
- cement-based composites /
- dry-wet circulation /
- compressive strength /
- mechanism analysis /
- stability
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圖 1 不同干濕循環次數“飽水”狀態下應力?應變曲線
Figure 1. Stress?strain curves under "saturated" state in different dry?wet cycles
圖 2 不同干濕循環次數“失水”狀態下應力?應變曲線
Figure 2. Stress?strain curves under the condition of "water loss" in different dry?wet cycles
圖 3 不同干濕循環次數試件峰值強度與殘余強度. （a）“飽水”狀態；（b）“失水”狀態
Figure 3. Peak intensity and residual strength of samples under different dry?wet cycles: （a） state of "water saturation"；（b） state of "water loss"
圖 4 不同干濕循環次數試件單軸壓縮破壞形態
Figure 4. Different modes of samples after the uniaxial compression strength under different dry-wet cycles
圖 5 干濕循環12次不同狀態下水泥基復合材料X射線特征曲線. （a）風化層“失水”狀態；（b）風化層“飽水狀態”；（c）未風化層
Figure 5. XRD curves of cement-based composites under different conditions after twelve dry?wet cycles：（a）weathered layer under water-loss state；（b）weathered layer under saturated state；（c）unweathered layer
圖 6 干濕循環12次后未風化層不同放大倍數微觀形貌圖
Figure 6. SEM images of unweathered layer under different magnification after twelve dry?wet cycles
圖 7 干濕循環12次后風化層微觀形貌圖. （a）“失水”狀態；（b）“飽水”狀態
Figure 7. SEM images of microstructure after twelve dry-wet cycles：（a）water loss；（b）saturated state
表 1 水泥基復合材料成分及組成
Table 1. Composition of cement-based materials
組分 半定量（質量分數） A ${\rm{CaO}} \cdot 3{\rm{A}}{{\rm{l}}_2}{{\rm{O}}_3} \cdot {\rm{CaS}}{{\rm{O}}_4}(76\% )\;{\rm{2CaO}} \cdot {\rm{Si}}{{\rm{O}}_2}(24\% )$ A-A ${\rm{N}}{{\rm{a}}_2}{\rm{C}}{{\rm{O}}_3}(6\% )\;{\rm{Si}}{{\rm{O}}_2}(69\% )\;{\rm{BaBi}}{{\rm{O}}_3}(25\% )$ B ${\rm{CaS}}{{\rm{O}}_4}(61\% )\;{\rm{CaC}}{{\rm{O}}_3}(12\% )\;{\rm{CaS}}{{\rm{O}}_4} \cdot 2{{\rm{H}}_2}{\rm{O}}(27\% )$ B-B ${\rm{Si}}{{\rm{O}}_2}(70\% )\;{\rm{CaS}}{{\rm{O}}_4}(30\% )$ 
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表 2 不同干濕循環次數水泥基復合材料基本物理參數
Table 2. Basic physical parameters of cement-based materials under different dry-wet cycles
狀態 干濕循環
次數失水率/
%含水率/
%容重/
(kN·m?3)干容重/
(kN·m?3)“飽水” 0 0 71.8 11.5 3.2 1 3.4 70.9 10.9 3.2 3 2.5 71.1 11.1 3.2 6 2.8 71.3 11.1 3.2 9 4.5 70.2 10.4 3.2 12 9.8 69.2 10.4 3.2 “失水” 1 10.6 68.5 10.1 3.2 4 10.7 67.4 9.8 3.2 7 10.4 68.9 10.2 3.2 10 10.9 68.7 10.3 3.2
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表 3 不同干濕循環次數下水泥基復合材料單軸壓縮試驗結果
Table 3. Uniaxial compression test results of cement matrix composites under different dry?wet cycles
狀態 干濕循環次數 干濕時間/d 平均峰值強度/MPa 劣化度/% 平均殘余強度/MPa 平均彈性模量/MPa 養護完成 0 0 0.88 0 0.65 170 “失水” 1 1 0.80 9.0 0.50 123 “飽水” 1 2 0.89 ?11.3 0.63 130 “飽水” 3 6 0.94 ?5.6 0.59 123 “失水” 4 7 0.87 7.4 0.33 136 “飽水” 6 12 0.95 ?9.2 0.41 118 “失水” 7 13 0.83 12.6 0.27 145 “飽水” 9 18 0.96 ?15.7 0.42 116 “失水” 10 19 0.83 13.5 0.24 151 “飽水” 12 24 0.85 ?2.4 0.57 101
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表 4 干濕循環12次后不同狀態下水泥基復合材料主要礦物組成表
Table 4. Mineral composition of cement-based composites under different conditions after twelve dry?wet cycles
狀態 礦物名稱 化學式 “失水”狀態 碳酸鈣 ${\rm{CaC}}{{\rm{O}}_{\rm{3}}}$ “飽水”狀態 碳酸鈣 ${\rm{CaC}}{{\rm{O}}_{\rm{3}}}$ 碳硫硅鈣石 ${\rm{C}}{{\rm{a}}_{\rm{3}}}{\rm{Si}}{({\rm{OH}})_6}({\rm{C}}{{\rm{O}}_3})({\rm{S}}{{\rm{O}}_4}) \cdot 12{{\rm{H}}_{\rm{2}}}{\rm{O}}$ 鈣礬石 ${\rm{C}}{{\rm{a}}_{\rm{6}}}{\rm{A}}{{\rm{l}}_{\rm{2}}}{({\rm{S}}{{\rm{O}}_4})_3}{({\rm{OH}})_{12}} \cdot 2{\rm{6}}{{\rm{H}}_{\rm{2}}}{\rm{O}}$ 未風化層 鈣礬石 ${\rm{C}}{{\rm{a}}_{\rm{6}}}{\rm{A}}{{\rm{l}}_{\rm{2}}}{({\rm{S}}{{\rm{O}}_4})_3}{({\rm{OH}})_{12}} \cdot 26{{\rm{H}}_{\rm{2}}}{\rm{O}}$ 碳酸鈣 ${\rm{CaC}}{{\rm{O}}_{\rm{3}}}$ 碳硫硅鈣石 ${\rm{C}}{{\rm{a}}_{\rm{3}}}{\rm{Si}}{({\rm{OH}})_6}({\rm{C}}{{\rm{O}}_3})({\rm{S}}{{\rm{O}}_{\rm{4}}}) \cdot 12{{\rm{H}}_{\rm{2}}}{\rm{O}}$ 其他 —
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