3.3.1. Hot-Dry Environment
In order to analyze the effect of a hot-dry environment on the microstructure of cementitious materials, the specimens of FA0-P were cured under the conditions of SC and HD to 28 d and then used to perform the SEM, XRD, and TG-DTG tests.
Figure 6 shows the microstructure of FA0-P under the SC and HD curing systems. As can be seen from
Figure 6a, under the condition of SC, the internal structure of paste is compact. As can be seen from
Figure 6b, under the condition of HD, the internal structure of cement paste is loose and porous, and the distributions of hydration products are uneven. Large hexagonal lamellar CH (calcium hydroxide) crystals exist in hydration products. The loose and porous internal structure is an important reason for the sharp decline in the mechanical strength of mortar under the condition of HD.
Figure 7 shows the XRD test results of FA0-P under the SC and HD curing systems. It can be seen from
Figure 7 that hydration products under the SC condition are mainly CH crystals, Aft, and unhydrated C
2S. However, under the HD condition, the hydration products are mainly CH crystals, unhydrated C
2S (Dicalcium silicate), and C
3S (Tricalcium silicate); Aft (Ettringite) is not found. Moreover, the diffraction peak intensity of CH under the SC condition is higher than that under the HD condition. This shows that compared with the SC condition, lots of cement at 28 d is still not hydrated under the HD condition, leading to the deterioration of mortar performance.
Figure 8 shows the thermal analysis test results of FA0-P under the SC and HD curing systems. As shown in
Figure 8, under different curing systems, the trend of the curves is basically the same, but there is a great difference in the peak intensity. This indicates that the hydration products of FA0-P under the SC and HD curing systems are basically the same, but the contents of the hydration products are different. Three peaks can be clearly seen in
Figure 8. The endothermic peaks between 80 °C and 200 °C are generated by the dehydration of ettringite, AFm, and CSH gel. The endothermic peaks at about 460 °C are mainly caused by the decomposition of hydration product CH. The decomposition peaks of calcium carbonate are about 700 °C. The endothermic peaks of CSH gel and CH under the HD condition are significantly lower than those under the SC condition, indicating that the number of hydration products of cement under the HD condition is significantly less than that under the SC condition. This is consistent with the XRD test results; that is, the hydration degree of cement under the HD condition is low.
From the above microscopic tests, it can be known that under the condition of SC, the hydration reaction can proceed normally and the degree of hydration is high at 28 d. Therefore, the internal structure of paste is compact. However, under the hot-dry environment, water on the surface of the specimen evaporates faster than standard curing. The internal structure can still carry out the hydration reaction, but the degree of hydration is low. The high temperature can accelerate the early hydration reaction rate of cement. The early hydration rate is too fast to allow the hydration products to diffuse in time, resulting in hydration products accumulating irregularly on the surface of cement particles. Therefore, the hydration reaction rate becomes slow and even stops when the uneven hydration products cover the surfaces of the cement particles. Furthermore, under the hot-dry condition, the rapid evaporation of water will seriously affect the further progress of the hydration reaction. The hot-dry condition could not change the kind of hydration products, but it can result in the uneven distribution of hydration products, which has a great influence on the degree of hydration. As a result, under hot-dry condition the inner structure of paste is loose and porous.
3.3.2. Film Curing Time
Fly ash is a kind of mineral admixture with pozzolanic activity. When cement is mixed with fly ash, fly ash particles will undergo a secondary hydration reaction [
21,
22]. A secondary hydration reaction is the reaction of calcium hydroxide (CH) produced by cement hydration with the active component of fly ash to produce new hydration product. A secondary hydration reaction will increase the content of hydration products and refine the pore structure of the cement paste [
23,
24,
25,
26,
27,
28]. The activity of fly ash is more easily activated at a high temperature, which is conducive to the secondary hydration reaction. However, the process of the secondary hydration reaction is also slow. From the previous mechanical experiments, it can be seen that the strength of FA25 -M under the film curing condition is the best (
Figure 5). In order to study the influence of different curing systems (film curing time) on cement-fly ash mortar, the specimens of FA25-P group were cured under different curing systems to 28 d and used to perform SEM, XRD, and TG-DTG tests.
Figure 9 shows the SEM pictures of FA25-P under the SC condition. As can be seen from
Figure 9a,b, under the condition of SC, a large number of hydration products are generated and distributed evenly. The fly ash particles inside the paste have taken part in the hydration reaction. The internal structure of paste is compact, and there are some hydration products attached on the surface of the fly ash.
Figure 10 shows the pictures of SEM of FA25-P under the HD condition. As can be seen from
Figure 10a, under the HD condition, the hydration products in the paste are loose. The distribution of hydration products is uneven, and the porosity is obviously higher than that under the condition of SC.
Figure 10b shows that, under the condition of HD, there are some hydration products on the surface of fly ash, but the distribution of hydration products around the fly ash particles is uneven, and there are many pores around the fly ash particle.
Figure 11,
Figure 12 and
Figure 13 respectively show the SEM pictures of FA25-P under FC1–FC3 conditions. By comparing
Figure 11,
Figure 12 and
Figure 13, it can be seen that the microstructure of paste under the FC1 condition is compacter than HD, but there are still many pores, and the irregular accumulation of hydration products can be observed clearly. Under the FC2 condition, the compactness of paste is improved, but the distribution of hydration products is still uneven. Under the FC3 condition, the compactness of the structure is significantly improved, and the porosity is significantly reduced. Therefore, with the increase in film curing time, the compactness of internal structure is enhanced. It can be observed from
Figure 10b,
Figure 11b,
Figure 12b and
Figure 13b that hydration products are attached on the surface of fly ash under different curing systems. It shows that the hydration reaction of fly ash occurs under the hot-dry environment, and the activity of fly ash is stimulated by the high temperature. However, the degree of hydration reaction of fly ash is different under different film curing times. It can be seen from
Figure 13b that the hydration reaction of fly ash particles is almost fully under the condition of FC3.
Figure 14 shows the XRD test results of FA25-P cured to 28 d under different curing systems. As can be seen from
Figure 14, the types of hydration products under different curing systems are almost the same, but the peak intensity is different. Under the SC condition, the peak of AFt can be clearly observed, but under other curing systems, the peak of AFt is not obvious. The diffraction peak intensity of CH is the highest under the SC condition and the lowest under the HD condition. The content of CH under the conditions of FC1–FC3 is higher than that under the condition of HD, indicating that the early film curing is conducive to the further hydration reaction. The activity of FA is stimulated at a high temperature, which promotes the secondary hydration reaction between FA and CH and produces more hydration products. The
and
in fly ash react with the CH formed by cement hydration to produce hydrated calcium silicate, hydrated calcium aluminate, and other crystals [
29]. CH is consumed and the content of CH is reduced. As can be seen from
Figure 14, under the condition of FC, the CH content from low to high is FC3, FC2, and FC1. It shows that with the increase in film curing time, the content of CH gradually decreases; that is, the degree of secondary hydration was improved.
Figure 15 shows the TG-DTG test results of FA25-P cured to 28 d under different curing systems. Just as the result from
Figure 8, there are three obvious weight-loss plateaus in the TG curves for all conditions, corresponding to endothermic peaks in the DTA curves. The peaks between 80 °C and 200 °C are endothermic peaks generated by the dehydration of the AFm and C-S-H gel. The endothermic peaks at about 450 °C are mainly caused by the decomposition of CH. The endothermic peaks of CaCO
3 are between 600 °C and 720 °C. The mass loss from high to low is as follows: SC, FC3, FC2, FC1, and HD, and the difference between FC2 and FC3 is small. The DTG curves between 400 °C and 500 °C are too dense to distinguish clearly, so the enlarged figure is shown. It can be observed that the order of the size of the area enclosed by the DTG curve is also the same. This shows that with the increase in film curing time, the degree of hydration increases and the number of hydration products increases.
According to the above analysis, high temperatures can stimulate the pozzolanic activity of fly ash and promote the degree of secondary hydration reaction. The generated hydration products are filled in the pores and refine the pore structure. It is proved that film curing in the early stage in a hot-dry environment can effectively promote the degree of hydration reaction. Moreover, the microstructure becomes denser as the film curing time increases. Film curing and the addition of FA can improve the microstructure.