In this paper we present sol-gel synthesis and thermal and structural characterization of some lithium borophosphates. The as-prepared samples are mostly partially crystalline, and densification heat treatments at 500 °C cause samples to crystallize. In the phosphorus-rich part of the composition triangle we have lithium excess with respect to the nominal composition, which is likely due to the low reactivity of the phosphorus precursor. On the boron-rich side, in contrast, lithium losses are found which probably occur during syneresis.