3.3.2. Synthesis of IF-WS2 Nanoparticles from APT Precursor with H2S Gas

Six g APT were ultrasonically treated and dried before being placed into the centre of the quartz tube for the experiment (AHS1). Ar (50 mL/min) was flushed for 30 min before the furnace was switched on. H2S flowing was started from 550 °C till the end of the process, at a rate of 12 mL/min. The whole reaction lasted for 2 h at 800 °C, at a fixed Ar flow rate of 100 mL/min.

Except for experiments on various reaction times (summarised separately), all other experimental parameters are summarised in Table 2.


**Table 2.** Example parameters used for the synthesis of IF-WS2.

#### 3.3.3. Synthesis of IF-WS2 Nanoparticles WO3 and H2S Gas

The synthesis of WS2 nanomaterials from reaction of WO3 and H2S gas was similar to that from WO3 and S (Section 3.3.1), except for the H2 gas being replaced by H2S. The first trial was named experiment W1 (Table 2).


**Table 3.** Example parameters used for the synthesis of IF-WS2 with varying reaction times.

Table 3 summarises the parameters used for a series of experiment at a fixed rotation speed of 140 rpm, with reaction time varying from 10–170 min.

#### **4. Conclusions**

Based on the built rotary system, the large scale manufacture of IF-WS2 nanoparticles has been realised. Several synthesis methods have been studied, and the process starting with WO3 precursor and H2S reaction gas is most successful. Systematic studies have been carried out to optimise the parameters for IF-WS2 nanoparticle production, including precursor types, reaction temperatures, reaction time and reaction gases. Further refinements by modifying the working quartz tube and the feeding system have made the continuous manufacturing possible. This new technique, as a simple alternative to the fluidised bed method, has improved the yield of IF production from less than 1 g/batch using a traditional tube furnace to a few tens of g/batch. This process is easily scalable to industry production level, by incorporating existing equipment.

### **Supporting Information**

#### **1. Results and Discussion**
