For the N2 adsorption-desorption analysis, the unsupported
membranes were ground to form fine-powdered samples. N2
adsorption-desorption isotherms at 77 K were performed in
Micromeritics TriStar II 3020 equipment. The samples were previously
degassed, first at 90 C for 1 h and subsequently at 250 C for
5 h under N2 flow. The surface area values were obtained by
application of the BET equation. The calculation of the pore sizewas
performed by applying the NLDFT method. XRD patterns were
collected on a Rigaku MiniFlex diffractometer using Cu Ka radiation.
The XRD patterns, scanned with 2q values from 20 to 80, were
obtained using a step size of 0.02. TG-DTA analyses were performed
in a NETZSCH STA 449F3 instrument, heating the sample to
1100 C at a rate of 10 C/min under a 100 N mL/min air flow. The
surface microcosmic morphologies of the prepared membranes
were visualized with a field-emission scanning electron microscope
(FESEM), obtained with a Hitachi S4800 scanning microscope
operating at an accelerating voltage of 5 kV. Transmission electron
microscopy (TEM) analyses were performed on a JEOL 1011 microscope
operating at 200 kV. The particle size distribution of the
boehmite sols and the zeta potential of powders were characterized
by dynamic light scattering (DLS) in a Microtrac Zetatrac analyzer.
The temperature was kept constant at room temperature. The
refractive index of the g-alumina membranes fabricated on the
silicon substrates were measured with a J. A. Woollam Complete
EASE M2000U spectroscopic ellipsometer with a 632.8 nm laser
at a 70 incident angle [25].