3.1. XRD, EDX, ATD and ATG analysis
The mineral composition of the soil was examined using X-ray diffraction analysis (see Fig. 7). This technique is based on the analysis of diffraction patterns into d-spacing values, which are distinctive for each mineral, thereby facilitating their identification. The analysis revealed that the soil sample contained calcite and quartz, as indicated by the high peaks in the sample spectra. Additionally, the soil sample exhibited significant dolomite presence: dolomite with the chemical formula (CaMg(CO3)2). Finally, XRD analysis indicated the presence of muscovite (H2KAl3Si3O12) in the soil, as documented in Table 2.
Table 2
Results of DRX soil studied
Compound Name
|
Chemical Formula
|
Sample and mineral percentages (%)
|
Calcite
|
Ca(CO3)
|
43.33
|
Quartz
|
SiO2
|
36.51
|
Dolomite
|
CaMg(CO3)2
|
16.18
|
Muscovite
|
H2KAl3Si3O12
|
3.98
|
The X-ray diagram of kaolin is shown in Fig. 8. From the analysis (XRD), it was observed that kaolin powder is composed mainly of Quartz low (SiO2) and Illite [(K,H3O) Al2Si3Al O10 (OH)2]. Moreover, there is a small amount of Clinochlore, ferrien [(Mg,Fe,Al)6 (Si,Al)4 O10 (OH)8]. Table 3 presents a summary of the results of DRX analysis.
Table 3
Analysis results of DRX of kaolin powder studied
Compound Name
|
Chemical Formula
|
Sample and Mineral percentages (%)
|
Quartz low
|
Si O2
|
68.3
|
Illite
|
(K, H3 O) Al2 Si3 Al O10 (O H )2
|
30.1
|
Clinochlore, ferrien
|
( Mg, Fe, Al )6 ( Si, Al )4 O10 ( O H )8
|
1.6
|
The analysis of infrared (IR) spectra is particularly important to complete the physicochemical characterization of the samples studied. Based on the data in Fig. 9 and [31], an absorption band was observed between 3200 and 3800 cm− 1, which was associated with the stretching vibrations of the internal hydroxyl (OH) groups. In the soil sample studied, the absorption band is located at a wave number of 3400 cm− 1. The OH bond is found in both Muscovite and Dolomite, while the Si-O bond indicates the presence of quartz. Additionally, the Si-O-Al bond is present in Muscovite and Calcite. These findings reveal the presence of different elements and compounds within the soil samples, which contribute to their distinct spectral features.
In Fig. 10, different parts are observed. The first part shows bands from 3623 cm− 1 to 3393 cm− 1, these bands are due to vibrations of the O-H bonds of the hydroxyl groups in the sample [32]. In the second part, four bands of absorption were oberserved, the bands from 1643 cm− 1 to 1385 cm− 1 originate from the vibrations of Si-O bond in kaolin. In addition, the bands from 1069 cm− 1 to 1024 cm− 1 are due to symmetrical and asymmetrical stretching of the Si-O-Si bonds, respectively [32]. In the third part, bands from 795 cm− 1 to 692 cm− 1 correspond to different vibrations of Si-O-AlIV bonds (Al is four times coordinated) [33]. In the fourth part, two absorption bands with vibrations from 529 cm− 1 to 469 cm− 1, these vibrations are linked to Si-O-AlVI (Al is six times coordinated) and deformed Si-O-Si bonds, respectively [33].
SEM (Scanning Electron Microscope) images of the Errachidia soil studied are shown in Fig. 11.
The presence of randomly dispersed clay sheets was observed, which appeared in various forms such as elongated or rolled shapes, as well as in the form of sticks. Additionally, a few aggregates were also noted, and these may have resulted from impurities present in the clay.
The composition of a soil sample studied was examined using energy dispersive X-ray (EDX) analysis. The results revealed that the sample contained mainly silicon (Si), calcium (Ca), oxygen (O) and aluminum (Al) (Fig. 12). These results are consistent with the findings of X-ray diffraction (XRD) analysis, which showed the presence of quartz (SiO2) and calcite (CaCO3) in the soil sample. In addition, the detection of various other elements, including Al, K, Mg, Fe, Cl, O, C, Ca, Si, Ti and Na, in different concentrations in the soil samples, confirms the idea that the region concerned by the study is rich in a diverse range of muscovite type materials. The results of EDX analysis are presented in Table 4.
Table 4
Analysis results of EDX soil studied.
Element
|
Weight %
|
Atom %
|
C
|
5.01
|
8.26
|
O
|
54.47
|
67.45
|
Na
|
0.40
|
0.34
|
Mg
|
1.93
|
1.57
|
Al
|
5.79
|
4.25
|
K
|
1.78
|
0.90
|
Ti
|
0.47
|
0.19
|
Fe
|
3.66
|
1.30
|
Ca
|
14.00
|
6.92
|
Cl
|
0.10
|
0.06
|
Si
|
12.41
|
8.75
|
Total
|
100.00
|
100.00
|
Figure 13 shows EDX results for kaolin powder and the corresponding spectra for the nine peaks. The main elements detected in the sample are silicon, aluminum, carbon and oxygen, and some magnesium. EDX peaks of the kaolin sample indicate that kaolin contains just nine elements, namely C, O, Mg, Al, Si, Ti, Na, K, Fe, with contents of 17.39%, 50.09%, 0.61%, 8.80%, 17.11%, 0.48%, 0.54%, 1.84% and 1.13%, respectively. EDX results are summarized in Table 5.
Table 5
Analysis results of EDX kaolin studied.
Element
|
Weight %
|
Atom %
|
C
|
10.74
|
17.39
|
O
|
42.83
|
52.09
|
Na
|
0.64
|
0.54
|
Mg
|
0.77
|
0.61
|
Al
|
12.21
|
8.80
|
Si
|
24.70
|
17.11
|
K
|
3.70
|
1.84
|
Ti
|
1.18
|
0.48
|
Fe
|
3.24
|
1.13
|
Total
|
100.00
|
100.00
|
Figure 14 shows the scanning electron microscope (SEM) images of the kaolin powder. In order to visualize the internal morphology of the kaolin powder under the SEM microscope, a grayed background was observed. This amorphous background shows a few very fine particles, indicating the presence of a small quantity of Clinochlore.
The differential thermal analysis (DTA) and thermogravimetric analysis (TGA) were performed on the kaolin sample. The obtained DTA and TGA thermograms for the kaolin fraction are presented in Fig. 15. The TGA thermogram reveals three thermal phenomena:
- The endothermic peak around 60°C is caused by the departure of absorbed water located between the kaolin sheets [34].
- The exothermic peak observed at 448°C is characterized by the dehydroxylation of structural water, which is eliminated by a diffusion mechanism resulting in the formation of a new amorphous material, metakaolin [34]. The third exothermic peak observed at 622°C indicates the recrystallization of metakaolin [35].
- The ATG thermogram of this material shows two thermal phenomena: the first is mass loss (approx. 0.42%) corresponding to the evaporation of absorbed water. The second is mass loss (approx. 2.64%) which continues beyond 846°C, dehydroxylation due to the presence of Illite [36].
3.4. Mechanical strength of stabilized bricks
The measurement results for tensile and compressive strength are shown in Table 8.
Table 8
Tensile and compressive strength of studied samples
Pourcentage de géopolymère (%)
|
Rt en MPa
|
Rc en MPa
|
0
|
0.114
|
0.892
|
3
|
0.132
|
1.146
|
4
|
0.285
|
1.273
|
5
|
0.413
|
2.675
|
6
|
0.624
|
4.076
|
According to the results presented in Fig. 19 and Fig. 20, both tensile and compressive strength increase with an increase in the percentage of geopolymer in stabilized bricks. when the geopolymer content is at 6%, the bricks exhibit a remarkable increase in mechanical robustness. The compressive strength, represented by Rc(6% GP), is found to be 4.56 times the strength of bricks without geopolymer content [Rc(0%GP)], reflecting a 356% increase in the ability of the material to resist crushing loads. Similarly, the tensile strength, denoted as Rt(6%GP), reaches a value that is 5.47 times that of the non-geopolymerized bricks [Rt(0%GP)], indicating a 447% enhancement in resistance to tension. These multiplicative factors are not merely incremental but signify a substantial amplification in strength, suggesting that the geopolymer contributes significantly to the soil matrix's cohesion and overall durability. Moreover, these results may imply that geopolymers could be a viable alternative to traditional binders, offering enhanced mechanical properties that could be beneficial for sustainable construction practices. The increased strength with geopolymer addition could lead to the use of less material for the same structural requirements, reducing the environmental footprint.
The geopolymer contains elements such as silicon, aluminum, calcite and oxygen, which can reinforce the earth matrix and improve its tensile and compressive strength. In addition, the crystalline structure of the geopolymer contributes to a better cohesion of the earth and geopolymer particles, which can also reinforce the mixture and improve its mechanical strength. It is also possible that the porosity of the mixture has an impact on its tensile and compressive strength. Indeed, an earth matrix with higher density and lower porosity may be more resistant to mechanical stress than one with higher porosity. Indeed, as the addition of geopolymer to the earth mixture reduces the porosity of the mixture, this could also contribute to better mechanical strength.