In situobservation of the pressure-induced mesophase for 4′-n-hexadecyloxy-3′-nitrobiphenyl-4-carboxylic acid

In situ observation of the optical texture, and X-ray patterns of the pressure-induced mesophase seen for 4′-n-hexadecyloxy-3′-nitrobiphenyl-4-carboxylic acid (ANBC-16) was performed under hydrostatic pressures up to 100MPa using a polarizing optical microscope equipped with a high pressure hot stage and a wide angle X-ray diffractometer equipped with a high pressure vessel respectively. It was found that the pressure-induced mesophase (hereafter refered to as ‘X’) appeared at pressures above 60 MPa, and exhibits a birefringent broken-fan or a sand-like texture that remain unaltered in the SmC phase. The POM-transmitted light intensity curve measured on heating clearly showed the Cr4 → Cr1 → SmC → ‘X’ → SmA → I transition sequence at 80 MPa. The optical texture and the POM-transmitted light intensity measured during a pressure cycle at 185°C showed a reversible change between the cubic and ‘X’ phases. The WAXD pattern of the ‘X’ phase showed a spot-like pattern, suggesting no layered structure for this phase, and also revealed a substantial decrease in the d-spacing of the low angle reflection at 80 and 100 MPa, compared with the d-spacings of the (0 0 1) reflection of the SmC phase and also the (2 1 1) reflection of the cubic phase. It is concluded from these data that the ‘X’ phase is a birefringent hexagonal columnar phase.