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Hydroxyapatite–poly(vinyl alcohol) composite blocks were produced by freeze–thawing in situ synthesized hybrid suspension. Matrix mediated precipitation of hydroxyapatite particles in the polymer, controlled the particle size in nanometer range (<100nm) and hydrogelation induced an ordered three-dimensional assembly of the particles. Morphological and crystallographic characterization revealed the formation of a macro-porous hydroxyapatite–poly(vinyl alcohol) nanocomposite block. Initial results indicate compositional dependence of modulus of elasticity of the composite.