The aim of this paper was to verify a
possible correlation between the pore-size of meso-
porous silica nanoparticles (MSNs) and the sizes of
gold nanoparticles (AuNPs) obtained by an impreg-
nation of gold(III) chloride hydrate solution in the
MSNs, followed by a specific thermal treatment.
Mesoporous silica nanoparticles with tunable pore
diameter were synthesized via a surfactant-assisted
method. Tetraethoxysilane as silica precursor, cetyl-
trimethylammonium bromide (CTAB) as surfactant
and toluene as swelling agent were used. By varying
the CTAB–toluene molar ratio, the average dimension
of the pores could be tuned from 2.8 to 5.5 nm.
Successively, thiol groups were grafted on the surface
of the MSNs. Finally, the thermal evolution of the gold
salt, followed by ‘‘in situ’’ X-ray powder diffraction
(XRPD) and thermogravimetric analysis (TGA),
revealed an evident correlation among the degradation
of the thiol groups, the pore dimension of the MSNs
and the size of the AuNPs. The samples were
characterized by means of nitrogen adsorption–
desorption, transmission electron microscopy, small-
angle X-ray scattering, XRPD ‘‘in situ’’ by synchro-
tron radiation, and ‘‘ex situ’’ by conventional tech-
niques, diffuse reflectance infrared Fourier transform
spectroscopy, and TGA