The synthesis of zirconium oxide with a mesostructured framework (Zr-T
MS) has been achieved through the use of amphiphilic compounds with a
variety of headgroups (anionic and nonionic) and tail group chain leng
ths (1-18 carbons). Anionic surfactants with phosphate, carboxylate, s
ulfate, and sulfonate headgroups led to disordered hexagonal and/or la
yered phases. Mesoporous zirconia with high surface areas could be obt
ained through calcination of materials templated with phosphate amphip
hiles; the phosphate headgroups remained on the pore walls and appeare
d necessary for thermal stability. Nonionic amine amphiphiles have bee
n found to lead to less ordered zirconia mesostructures, due to the we
ak interaction with the zirconium n-propoxide precursor. The chain-len
gth-independent templating ability of the amphiphiles and ex situ P-31
MAS NMR of dodecyl phosphate (before and after incorporation into Zr-
TMS) supported a method of formation involving covalent-bond interacti
ons between the headgroup and the inorganic precursor.