2.3.2. SEM Characterization

Microstructure of samples was further monitored by SEM. As can be seen from Figure 3, both TS-1 and Ni-TS-1 samples showed uniform spherical particles with the size of about 0.1–0.2 μm. Compared with TS-1, the size and shape of Ni-TS-1 did not have an obvious change. These results showed that the metal oxide did not destroy the crystal structure of TS-1, nor did it change the morphology of TS-1 particles.

**Figure 3.** SEM images of TS-1 (**A**) and 3 wt % Ni-TS-1 (**B**).

2.3.3. Induced Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) and N2 Adsorption-Desorption Characterization

The results of ICP-AES for the XNi-TS-1 catalyst are shown in Table 4. The loading efficiency (*e*) of Ni on TS-1 was about 70%.


**Table 4.** Ni content, specific surface area, and micropore volume of TS-1 and XNi-TS-1.

N2 adsorption–desorption isotherm of TS-1 and XNi-TS-1 are shown in Figure 4. According to the BDDT classification, all of the samples showed type IV isotherms with type H3 hysteresis loop, indicating the presence of mesopores. In addition, the introduction of Ni did not affect the presence of mesopores in TS-1. As shown in Table 4, the decrease in surface area and pore volume can be observed with the increase of Ni dosage. The N2 adsorption capacity of the Ni-TS-1 decreased compared to TS-1. This suggested that the metal oxides partially occupied the microporous channels.

**Figure 4.** N2 adsorption–desorption isotherm of TS-1 and XNi-TS-1.
