Small-angle X-ray scattering and rheological studies on the ordering process of cylindrical microdomains in a polystyrene-block-polyisoprene copolymer

Hashimoto, Takeji; Ogawa, T.; Sakamoto, Naoki; Ichimiya, Makoto; Kim, Jin Kon; Han, Chang Dae

doi:10.1016/s0032-3861(97)00442-4

Cited by 24 publications

(27 citation statements)

References 34 publications

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“…This suggests that it be not necessary to have the same results for SAXS and rheology. However, Balsara et al 36) and Hashimoto et al 10) showed that the grain size has only little effect on the elastic modulus. Therefore, the good agreement between the experimental results from SAXS and rheology (Fig.…”

Section: Resultsmentioning

confidence: 99%

“…Numerous studies have been reported on the order-disorder transition (ODT) in block copolymers during the past two decades 1,2) . However, although the ordering process of microdomains in a block copolymer from a disordered state to ordered states has been studied very recently, the mechanism is not fully understood [3][4][5][6][7][8][9][10][11][12] . Floudas et al 3) found that the ordering process of a polystyrene-blockpolyisoprene (SI) copolymer can be described by an Avrami-type nucleation and growth mechanism, and this depended on the quenching depth (DT), namely, the distance between T ODT and the phase-separating temperature.…”

Section: Introductionmentioning

confidence: 99%

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Ordering kinetics of cylindrical and spherical microdomains in an SIS block copolymer by synchrotron SAXS and rheology

Kim

Lee

Ree

et al. 1998

Macromol. Chem. Phys.

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The ordering kinetics of cylindrical and spherical microdomains in a polystyrene-block-polyisoprene-block-polystyrene (SIS) copolymer were studied using synchrotron small-angle X-ray scattering (SAXS) and rheology upon quenching the sample from a disordered state to an ordered state having either spherical or cylindrical microdomains. The SIS exhibits an order to order transition at -181 "C, a lattice disordering transition at -21OOC and becomes disordered at higher temperatures. Higher order peaks in the SAXS profiles corresponding to hexagonally packed cylindrical (HEX) microdomains appeared after less than 1 h when the sample was quenched from 235°C to 170°C. When quenched from 235°C to 200°C, a broad higher order peak at -1.65 qm, corresponding to spheres with liquid-like short-range order, was persistent up to 4 h before higher order peaks corresponding to body-centered cubic (BCC) microdomains appeared. We repeated this experiment by changing temperature from one ordered state with BCC microdomains to another with HEX microdomains, and vice versa. The BCC microdomains were attained within 1 h when heating from 170 "C to 200 "C. The transition between HEX and BCC is thermoreversible. The time evolution of dynamic storage modulus G' is in good agreement with that of SAXS intensity.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Ordering kinetics of cylindrical and spherical microdomains in an SIS block copolymer by synchrotron SAXS and rheology

Kim

Lee

Ree

et al. 1998

Macromol. Chem. Phys.

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“…morphologies, particularly in thin films. A number of schemes, including shear, 7 electric fields, 2 thermal gradients, 8,9 solvent annealing, 10 flow, 11 graphoepitaxy, [12][13][14] and chemical prepatterning, 15,16 have been proposed to improve the ordering of BCP domains. Among these different possibilities, the graphoepitaxy based on prepatterned templates is one of the most used techniques to form large-scale perfectly ordered patterns in thin films.…”

Section: Introductionmentioning

confidence: 99%

Ordering kinetics of block copolymers directed by periodic two-dimensional rectangular fields

Xie

Qiu

et al. 2011

The Journal of Chemical Physics

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The ordering kinetics of directed assembly of cylinder-forming diblock copolymers is investigated by cell dynamics simulation of the time-dependent Ginzburg-Landau theory. The directing field, mimicking chemically or topologically patterned surfaces, is composed of a rectangular array of potential wells which are attractive to the minority blocks. The period of the templating fields is commensurate with the hexagonal lattice of the block copolymer domains. The ordering kinetics is described by the time evolution of the defect concentration, which reveals that the rectangular field of [1 m] for a given density multiplication has the best directing effect, and the reversed case of [m 1] has the worst. Compared with a hexagonal directing field, the rectangular field provides a better directing efficiency for a fixed high density multiplication. The difference of the directing effect can be understood by analyzing the ordering mechanisms in the two types of directing fields. The study reveals that the rectangular pattern is an alternative candidate to direct block copolymer assembly toward large-scale ordered domains.

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“…Over the past fifteen years, several revealing studies of block copolymer ordering kinetics have been described. Measurements have been made on the lamellar,11–16 hexagonally‐packed cylinders,17–23 bicontinuous gyroid,24 and body centered cubic packed (BCC) spherical micelle25–30 phases, all on forming from the disordered state. These order–disorder transitions (ODTs) have been characterized using time‐resolved small angle X‐ray scattering (tr‐SAXS),11, 17, 18, 25–27, 31–33 rheology,12, 13, 17–19, 26 depolarized light scattering,14, 20–23, 34 transmission electron microscopy (TEM),15, 28, 35 and polarized optical microscopy (POM) 24, 36, 37.…”

Section: Introductionmentioning

confidence: 99%

Grain shapes and growth kinetics during self‐assembly of block copolymers

Chastek

Lodge

2005

J Polym Sci B Polym Phys

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ABSTRACT:With block copolymer equilibrium phase behavior becoming increasingly better understood, a more detailed description of ordering kinetics is feasible. This article highlights recent experimental observations that provide new insight into ordering kinetics and grain structures when a block copolymer liquid is first cooled below the order-disorder transition. Measurements have been made on several concentrated poly(styreneb-isoprene) solutions, with concentrations and temperatures adjusted to access the cylinder, lamellar, and gyroid phases. A diverse set of grain types were observed using polarized optical microscopy (POM). Cylinder grains were either oblate ellipsoids or spherulites, whereas the lamellar phase formed prolate ellipsoidal grains, twinned ellipsoidal grains, twofold twinned grains, and spherulites. The orientation of the cylinders and lamellae within the grains were unambiguously identified. The shapes of the ellipsoidal and twinned grains were dictated by the relative interfacial tensions of the available growth surfaces with respect to the disordered state. Grain growth front velocities were also quantified before grain impingement, and consistent values were obtained among different grains for a given sample and quench temperature. The experimental growth velocities were compared to an expression derived by Goveas and Milner. There was good agreement in terms of the temperature dependence, and the absolute magnitude was predicted with some success. The rates of nucleation and overall conversion to the ordered phase were also determined.

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Small-angle X-ray scattering and rheological studies on the ordering process of cylindrical microdomains in a polystyrene-block-polyisoprene copolymer

Cited by 24 publications

References 34 publications

Ordering kinetics of cylindrical and spherical microdomains in an SIS block copolymer by synchrotron SAXS and rheology

Ordering kinetics of cylindrical and spherical microdomains in an SIS block copolymer by synchrotron SAXS and rheology

Ordering kinetics of block copolymers directed by periodic two-dimensional rectangular fields

Grain shapes and growth kinetics during self‐assembly of block copolymers

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