Sol-gel glasses with a composition close to KTiOPO4 (films & bulk gels) are synthesised from titanium propoxide, di-n-butyl phosphate, potassium acetate, tetraethoxysilane (TEOS) and 3-glycidoxypropyltrimethoxysilane. Thin films are drawn by dip coating. The annealing process consists of three steps: the evaporation of solvents, oxidation and removal of organics at 250 C and 350 C and the the crystallisation between 500C and 800C. The structure formation is observed by FTIR spectroscopy (Fourier-Transform Infrared spectroscopy) and Karl-Fischer coulometry. UV-vis spectroscopic investigations show; that the amount of Ti3+ ions increases with higher annealing temperatures and times. XRD measurements prove, that the crystallisation at least requires 600C. At SiO2 containing bulk samples only KTiOPO4 crystals are precipitated with an average diameter of 50nm.
