Ammonium bis(biureto)borate,
NH4[B(biu)2]
(biu = NH–(CO)–NH–(CO)–NH),
was synthesized as a phase pure powder from urea and triethylborate
in a sophisticated solvothermal process. Its crystal structure was
determined via single-crystal XRD and it crystallizes in its own structure
type in space group P2/c (a = 9.2855(3) Å, b = 4.8019(2) Å, c = 10.9008(4) Å, β = 110.757(2)°, Z = 2). NH4[B(biu)2] was characterized
with FT-IR and UV/vis spectroscopy as well as thermogravimetry. It
was identified as a crucial reaction intermediate during the boron
nitride synthesis from urea and boric acid. Mixtures of boric acid
and urea were studied via TGA and DSC, and furthermore, three series
of solid state reactions varying calcination temperature, time, and
ratio of starting materials were conducted in order to study the formation
and thermal decomposition of NH4[B(biu)2]. Based
on these experiments under careful comparison to our studies on the
properties of phase pure, solvothermally synthesized NH4[B(biu)2] we suggest a reasonable reaction sequence for
the formation of boron nitride starting from urea and boric acid.