Sol Gel Route
Sol Gel Route
Sol Gel Route
c 2003 Kluwer Academic Publishers. Manufactured in The Netherlands.
J. LLIBRE
Carburos Metálicos SA, R&D, Passeig de la Zona Franca 14-20, 08038 Barcelona, Catalunya, Spain
Abstract. A simple and versatile method to obtain silica aerogel particles based on the hydrolysis and subsequent
condensation of silicon alkoxides in supercritical fluids is proposed. This microparticle production route reduces
the number of steps of traditional microparticle sol-gel processing.
A case example is explained in more detail. Spherical and fiber silica morphologies were obtained by a one
step method using a sol-gel process with supercritical acetone as a solvent. Particle size was controlled by varying
the relative amounts of alkoxysilane, water and acetone. The resulting materials are influenced by a large number
of experimental parameters; it has been observed that a quite relevant one is the supercritical fluid venting rate.
The morphology of the particles was characterized by electron microscopy (SEM and TEM) and Atomic Force
Microscopy (AFM). Alternatively, a low temperature synthesis can be performed by using supercritical carbon
dioxide as solvent and formic acid as condensation agent.
investigated the influence of different synthesis param- Table 1. Mean particle size obtained by varying
eters and the conditions of the synthesis media on the the hydrolysis parameter, h.
structure and morphology of the obtained aerogel silica Sample h Particle size
particles.
A 2 1.2 µm
B 4 1.7 µm
Experimental
C 8 2.2 µm
Figure 1. (a) Referring to sample A. Scanning electron micrograph of aerogel spherical shape silica particles narrowly distributed in size,
particle diameter between 0.50 and 2 µm. (b) Fiber-like structure with a diameter of 75 nm and a length of some microns.
Direct Formation of Silica Aerogel Microparticles 647
Figure 2. (a) Sample C, SEM micrograph of the spherical particles and its particle size distribution. (b) Sample B, SEM micrograph and
particle size distribution.
the duration of the pressure release in all the exper- Results and Discussion
iments was of 30 min. The injection of liquids was
achieved through a very fine nozzle using a syringe In all the experiments a white dry powder was uni-
pump. formly distributed all over the walls and base of the
An alternative route to this one was to inject the reactor. No liquid was found, indicating a complete
reactives in liquid CO2 and dissolving the remaining reaction.
water and alcohols from the sol reaction in a continuous The apparent powder density was between
flow of liquid CO2 , then reach the CO2 supercritical 0.06 g/cm3 and 0.08 g/cm3 depending on the initial
parameters and venting the autoclave. parameters.
648 Moner-Girona et al.
Figure 4. Sample C, Surface of a microsphere by AFM. Lateral dimensions: (500 nm×500 nm). The gray scale corresponds to vertical
amplitude of 15 nm.
Direct Formation of Silica Aerogel Microparticles 649