In the present study, in-situ synthesis of carbon nanotube/hydroxyapatite nano composite powder with stable homogeneous dispersions of carbon nanotubes (CNTs) was carried out using surfactant as dispersing agent. By applying sol-gel method, dispersion in the hydroxyapatite matrix and its effects on the microstructure were investigated. The chemical and phase composition, structure and morphological and size analyses were performed using XRD, FT-IR, SEM, TEM/SAED/EDX, Raman, UV-Vis spectroscopy and differential scanning calorimetry (DSC). The influences of different dispersing agents (sodium dodecyl sulfate, SDS) as a benchmark for future dispersion experiments) and excitation wavelength are discussed and the results are compared to the commonly used UV-Visible spectroscopic analysis. The results indicated that synthesis of hydroxyapatite particles in the presence of the carbon nanotubes had the best homogenization of the carbon nanotube dispersion and faster crystallization of hydroxyapatite, and the use of SDS for dispersion carbon nanotubes at hydroxyapatite matrix rendered formation of hydroxyapatite coating on CNTs surface. The average crystallite size of heat-treated (at 600°C) samples, estimated by Scherrer,s equation, was found to be ~50-60 nm that was confirmed by TEM.