Diblock copolymers consisting of flexible polystyrene and semiflexible poly(n-hexyl isocyanate), P(S-b-HIC)s, were prepared by anionic polymerization, followed by size-exclusion chromatography (SEC) fractionation. Two P(S-b-HIC) samples having PHIC volume fractions (Φ_PHIC) of 0.18 and 0.31, sufficiently high molecular weights (M_n,PS and M_n,PHIC are both larger than 10 kg/mol), and narrow molecular weight distributions (M_w/M_n < 1.05) were obtained. The microphase-separated structures of the two P(S-b-HIC) samples were investigated by transmission electron microscopy (TEM) and small- and wide-angle X-ray scattering (SAXS and WAXS). TEM and SAXS show that both the P(S-b-HIC) samples exhibit hexagonally packed cylindrical structures but different cross-sectional shapes; namely, P(S-b-HIC)-0.18 has a round-shaped cross-section while P(S-b-HIC)-0.31 has a distorted cross-section. From the WAXS measurements, P(S-b-HIC)-0.31 exhibits a sharp peak at q* = 3.9 nm⁻¹, which is different from that of a nematic PHIC homopolymer that has a peak at q* = 4.6 nm⁻¹. These results indicate that the PHIC blocks in P(S-b-HIC)-0.31 align obliquely to the interface in the columnar domain.

由柔性聚苯乙烯和半柔性聚（正己基异氰酸酯）、P(S- b- HIC)组成的二嵌段共聚物通过阴离子聚合制备，然后通过尺寸排阻色谱 (SEC) 分级。两个 P(S- b -HIC) 样品的 PHIC 体积分数 ( Φ _PHIC ) 为 0.18 和 0.31，具有足够高的分子量（M _n,PS和M _n,PHIC均大于 10 kg/mol），以及窄分子获得了重量分布（M _w / M _n  < 1.05）。两种P(S- b)的微相分离结构-HIC) 样品通过透射电子显微镜 (TEM) 和小角度和广角 X 射线散射 (SAXS 和 WAXS) 进行研究。TEM 和 SAXS 表明两种 P(S- b- HIC) 样品都表现出六边形堆积的圆柱形结构，但横截面形状不同；即，P(S- b -HIC)-0.18 具有圆形截面，而 P(S- b -HIC)-0.31 具有扭曲截面。从 WAXS 测量结果来看，P(S- b -HIC)-0.31 在q * = 3.9 nm ^-1处显示出一个尖峰，这与在q * = 4.6 nm ^-1处有一个峰的向列型 PHIC 均聚物的峰不同. 这些结果表明 P(S- b-HIC)-0.31 与柱状域中的界面倾斜对齐。