A facile three step sol-gel-precipitation process is used to synthesize Mg(OH)2 nanowhiskers on micron-sized zeolite 5A particle surfaces at room temperature. The putative amorphous gelation product, Mg(OH) n(OR)2-n, forms first by a controlled hydrolysis and condensation reaction involving magnesium isopropoxide and water, ultimately leading to precipitation to form Mg(OH)2 structures on the zeolite surface. The optimum conditions for one dimensional Mg(OH)2 whisker formation are found to be six times the stoichiometric amount of water using 1 M HCl as the catalyst for the sol-gel reaction. The one-dimensional Mg(OH) 2 whiskers have an average diameter of 5-10 nm and length of 50-100 nm. The zeolite micropores are not affected by the Mg(OH)2 whiskers formed on the surface. The surface roughened zeolite 5A, with a Mg(OH) 2 content of about 9 wt%, showed improved adhesion between the zeolite and the polymer in a mixed-matrix composite membrane. © 2011 Springer Science+Business Media, LLC.