Page 127 - Book Hosokawa Nanoparticle Technology Handbook
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2.5 PORE STRUCTURE                                                           FUNDAMENTALS
                  bromide (C TMABr), one type of surfactant, forms  mesoporous material in which a liquid crystal tem-
                           16
                  a liquid crystal phase that is hexagonal, cubic, or  plate method is used. A self-organized mesostructure
                  lamellar in structure, depending on the solution  is formed by adding an inorganic precursor
                  conditions. A periodic pore-structure of mesoporous  (tetraethoxysilane, for example) to an aqueous solu-
                  materials is obtained by transferring the structure of  tion of a surfactant under appropriate conditions.
                  the liquid crystal onto an inorganic material. Figure  A mesoporous material with uniform pores can be
                  2.5.15 shows a scheme for the synthesis of a   synthesized by removing the surfactant from a
                                                                 mesostructured substance composed of a complex of
                                                                 the inorganic framework and the surfactant. Generally,
                                                                 a very low concentration of the surfactant is used for
                                                                 the synthesis of mesoporous material, in which the
                                                                 surfactant is present in the form of molecules or free
                                                                 micelles. The  mesoporous structure is believed to
                                                                 be formed by a co-operation of the surfactant and an
                                                                 inorganic molecules because a self-assembly of
                                                                 ordered mesostructure is induced by the addition of
                                                                 an inorganic precursor to a dilute surfactant solution
                  (a) 1D-channel structure  (b) 3D channel structure  [13]. Alkyltrimethylammonium chloride/bromide and
                                                                 tri-block copolymers are commonly used as a surfac-
                                                                 tant template.  A mesoporous silica (FSM-16) with
                                                                 higher stability can be synthesized using kanemite
                                                                 (NaHSi O ·3H O), a layered polysilicate, as the inor-
                                                                         5
                                                                       2
                                                                            2
                                                                 ganic precursor [2].
                                                                 (3) Synthesis of monodisperse particles
                                                                 There are various methods for synthesizing spherical
                                                                 monodisperse mesoporous particles.  The Stöber
                                                                 method is typically used, in which precipitation is
                                 (c) 3D cage structure           induced under alkaline conditions in a mixed solvent
                                                                 of water and alcohol [14–17]. A surfactant
                  Figure 2.5.14                                  (C H 2n 1 N(CH ) Br) and sodium hydroxide are
                                                                   n
                                                                             3 3
                  Pore-structures of ordered mesoporous materials.  dissolved in a mixed solvent of water and methanol,
                                   Inorganic
                                   precursor      Surfactant
                                                           Inorganic
                                                           monomer






                                                         Self-assembly


                              Surfactant/water
                                                         Framework
                                           Micelle                    2-30nm



                                 condensation                Removal of
                                                              surface

                                          Surfactant/inorganic           Mesoporous
                                             complex                     materials
                  Figure 2.5.15
                  Synthesis of ordered mesoporous material using surfactant as a template.

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