Nanocomposites of Poly(vinylidene Fluoride) with Organically Modified Silicate
We report a study of the impact of cold crystallization on the structure of nanocomposites comprising poly(vinylidene fluoride) (PVDF) and Lucentite STN{trademark} organically modified silicate (OMS). Nanocomposites were prepared from solution over a very wide composition range, from 0.01 to 20% OMS by weight. Thermal preparation involved cold crystallization at 145 degC of quenched, compression-molded plaques. Static and real-time wide and small angle X-ray scattering (WAXS, SAXS), Fourier transform infrared spectroscopy (FTIR), and differential scanning calorimetry (DSC) were used to investigate the crystalline phase of PVDF. For OMS content greater than 0.50 wt%, WAXS studies show that that the silicate gallery spacing increases modestly in the nanocomposites compared to neat OMS film, indicating a level of polymer intercalation. Using Gaussian peak fitting of WAXS profiles, we determine that the composition range can be divided into three parts. First, for OMS greater than 0.5 wt%, alpha phase fraction, {phi}{sub {alpha}}, is insignificant ({phi}{sub {alpha}}{approx}0-0.01). Second, at the intermediate range, for OMS between 0.5 wt% down to 0.025 wt%, beta phase dominates and the beta fraction,{phi}{sub {beta}}, is related to alpha by {phi}{sub {beta}}>{phi}{sub {alpha}}. Third, below 0.025 wt% OMS, alpha dominates and {phi}{sub {alpha}}>{phi}{sub {beta}}. The ability of small amounts of OMS ({le}0.025 wt%) to cause beta crystal domination is remarkable. Overall, crystallinity index (from the ratio of WAXS crystal peak area to total area) ranges from about 0.36 to 0.51 after cold crystallization. Real-time WAXS studies during heating of initially cold crystallized nanocomposites show that there is no inter-conversion between the alpha and beta phase PVDF crystals, where these crystals coexist at room temperature. While all samples showed a strong SAXS Bragg peak, indicating existence of two-phase lamellar stacks, the sample containing predominantly beta phase had poorly correlated lamellar stacks, compared to samples containing predominantly alpha phase.
- Research Organization:
- Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source
- Sponsoring Organization:
- Doe - Office Of Science
- DOE Contract Number:
- DE-AC02-98CH10886
- OSTI ID:
- 914321
- Report Number(s):
- BNL-78889-2007-JA; POLMAG; TRN: US200809%%24
- Journal Information:
- Polymer, Vol. 47, Issue 7; ISSN 0032-3861
- Country of Publication:
- United States
- Language:
- English
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