Single crystals of 1T-TaS2 were synthesized using the chemical vapor transport technique with I2 as the transport agent following the study of Inada et al. (32). Ta powder (Alfa Aesar, 99.97%) and S pieces (Sigma-Aldrich, 99.998%) were first mixed with a molar ratio of 1:2.02, heated to 970°C in an evacuated quartz tube, and subsequently quenched in cold water after 2 days. The resulting TaS2 powder was sealed with I2 again in an evacuated quartz tube and placed at the hot side of a temperature gradient from 920° to 820°C in a three-zone furnace for the chemical vapor transport process. After 2 weeks, the quartz tube was quenched in water to avoid the formation of the 2H phase. Thin layered crystals with a lateral size up to 1 cm could be found. Powder x-ray diffraction was performed to confirm that the obtained crystals were in the 1T phase.

An ultramicrotome fitted with a diamond blade was used to cleave 1T-TaS2 along the sulfur-sulfur plane (33), producing 50-nm-thick flakes of single crystals with an approximate dimension of 300 μm × 300 μm. Flakes were scooped from water onto standard TEM copper grids (300 lines/inch). The TEM grids were clamped to a copper holder, which was in good thermal contact with the cryostat cold head and the heater.

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