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Evaporation Induced Self-Assembly (EISA) of Block Copolymer Pluronic F-127 and Silica Using EtOH and THF

A. Ostrovsky, H. Sternlicht, A. Keller, G. L. Frey


Introduction
Si (OCH 2CH 3 ) 4 4 H 2O Si (OH ) 4 4 EtOH
hydrolysis

R3 Si (OH ) (OH ) Si R3 R3 Si O Si R3 H 2O
condensation

Objectives
To obtain the hexagonal phase of F127 and silica in both ethanol and THF solutions, on a flat surface. To examine the influence of confinement of these hexagonal phases within the channels of an AAM.

Mesostructured silica has an important role in novel applications. The type of mesostructure (hexagonal, cubic or lamellar) achieved from the EISA synthesis depends mainly on surfactant concentration and type and relative humidity during synthesis. Control over the orientation of the mesostrucutre can be achieved by confinement of the self assembly process to the pores of an anodic alumina membrane (AAM).

Experimental
Materials: Substrates: Polyimide and Anodized Alumina membranes (AAM) Precursor: TEOS Solvents: Ethanol and THF Surfactant: Pluronic F127.

Results and Discussion

EtOH
[111] [110]

THF
Figure 4: TEM images acquired from samples using THF, [F127]/[TEOS]=0.0114 molar ratio and 50% RH. A possible hexagonal mesustructure was received. Most pores were empty (as achieved in all the experiments using THF).
(1.3) (4)

5 6 4

(1 .1)

(1.2)

(2.1)

(2.2)

(3)

Figure 5: SAXS pattern acquired from polyimide films showing cubic mesostructure (Im3m) using THF, 90% RH, withdrawal rate of 2 [mm/sec] and [F127]/[TEOS]=0.0077 molar ratio. Using 60% RH, an ellipse pattern was achieved (figure not shown).

(5)

Figure 1: TEM images acquired showing three phases of cubic mesostructure (Im3m) using EtOH, [F127]/[TEOS]=0.0044 molar ratio and 50% RH. The pores are fully filled. 1.1-[111] zone axis showing {110} planes. 1.2- [110] zone axis showing {110} and {121} planes.1.3- [111], [110] zone axis, and an undefined phase implying phase transformation in process (into 3D hexagonal mesostructure). Figure 2: SAXS pattern acquired from polyimide films showing cubic mesostructure (Im3m) using EtOH, 50% RH and withdrawal rate of 2 [mm/sec]. 2.1- [F127]/[TEOS]=0.002 molar ratio. 2.2- [F127]/[TEOS]=0.00381 molar ratio. Cubic mesostructure is preferably achieved by [F127]/[TEOS]=0.002 on polyimide. Figure 3: SAXS pattern acquired from polyimide films using EtOH, 50% RH, withdrawal rate of 10 [mm/sec] and [F127]/[TEOS]=0.005 molar ratio showing an ellipse pattern indicating a poorly ordered film.
Figures 1.1, 1.2 d space no. Plane family 1 2 {110} 3 4 5 6 {110} {121}

The cubic mesostructure formed was characterized by the same typical parameters on both systems that were analyzed and matching experimental values achieved by other groups: d(110-SAXS)=12.74nm, d(110-TEM)=12.240.1nm, d(110-theoretical)~13nm.

Conclusions
o Hexagonal mesustructure was not achieved. o Cubic mesustructure was received on polyimide using both solvents. o Cubic mesostructure silica was achieved inside AAM using EtOH. The pore shape affects the phase observed. o We assume that hexagonal mesustructure can be achieved on polyimide using THF under the conditions: 60%<RH<90%, withdrawal rate of 2 [mm/sec] and [F127]/[TEOS]=0.0077.
RESEARCH POSTER PRESENTATION DESIGN 2011

References
Avigail Keller, Saar Kirmayer, and Tamar SegalPeretz, Gitti L Frey Langmuir, 10.1021/la203870. Yunfeng Lu et al, letters to nature, NATURE | VOL 389 | 25 SEPTEMBER 1997. Dongyuan Zhao et al, Adv. Mater. 1998, 10, No. 16 Grosso, D et al, A. Journal of Sol-Gel Science and Technology 2003, 26, 561-565.

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