## 3 Results
### Sem-Edx  
To evaluate the structures in terms of structure properties, SEM characterization was performed. SEM images reveal differences among the samples based on how the reduction occurs among the graphene sheets. Figure 4 shows SEM images of the modified samples (the blank, unmodified samples and smaller magnifications of the modified ones can be found in Figure S2). SEM images clearly show that the use of different modifying reagents alters the 3D structure of the final monolith. Different reagents result in different heteroatoms in the final structure, such as S, N, O, and Si. These heteroatoms can change the physicochemical properties of the material but also, and most importantly, the way graphene sheets are assembled during the reduction process. 3D materials prepared with the same amount of AsA and at the same temperature can give different 3D monoliths because of the heteroatoms present and the steric effects of these molecules among the graphene sheets. [41; 42]. Structures obtained at 60 \({}^{\circ}\)C seem more porous than those prepared at 90 \({}^{\circ}\)C.  
Nevertheless, this should be further evaluated through porosimetric measurements. Samples prepared at 90 \({}^{\circ}\)C and 0.5 AsA showed a more porous effect. For instance, TMON samples were more porous than TMOSN, which was less porous, and TMOS, more compact. The hydrophilicity of each component could play a role in the self-assembly of the sheets during reduction since some of the components can lead to more hydrophilic graphene that can result in a looser assembly. Similarly, TMON and TMOS samples prepared at 60 \({}^{\circ}\)C and 0.5 AsA displayed a quite similar morphology. On the contrary, TMOSN presented a quite porous morphology with defects on the sheets, as seen in the inlet of higher magnification from the SEM image in Figure 4i. The differences in morphology are SEM derived from both temperature and AsA quantity and the different compounds used for modification. The way they are stacking shows other aggregation degrees and hydrophobic interactions during the self-assembly of the modified graphene oxide platelets. For TMOS and TMON, the images are pretty similar, especially for temperatures at 60 \({}^{\circ}\)C. At 90 \({}^{\circ}\)C, the monolith modified with TMOS looks more compact with a low quantity of AsA and a little bit more porous with a higher reduction degree (due to more AsA). In the case of TMON, the results are similar, showing  
Figure 3: \({}^{13}\)C-NMR results for reduced graphene oxide monolith rGO60_0.5 modified with TMOS or TMON or TMOSN. a compact structure with less external porosity. The results for monoliths with TMOSN are pretty different, leading to porous monoliths, especially for 60 \({}^{\circ}\)C. In TMOSN, the more steric molecule probably helped create a more porous monolith (based on SEM images). The more hydrophobic TMOSN should have created a more porous structure since the modified platelets supposedly were more difficult to self-assemble due to their hydrophobic nature. In addition, with the other two compounds were more hydrophilic (especially TMON), and they were aggregating easier during the reduction of the chemical groups of the GO, leading to more compact structures. Nevertheless, the porosity results will reveal the real values of porosity. Interestingly, EDX measurements (Table 2) showed variations in percentages of S, Si, O, and N elements. The first three components have different analogies for S, Si, and O elements. TMOS has 1 Si, 3 O, and 1 S, TMON has 1 Si, 4 O, and 2 N. In addition, TMOSN has 1 Si, 3 O, 1 N, and 3 S. EDX results show that compared to the blank group, the group modified with TMOS has an increase in O (14%) as well as in percentages of Si and S. Adjusting the percentages of the elements with their molecular weights Si is 0.2 and S 0.18. An analogy of almost 1:1 in moles, similar to the initial structure.