The aim of the present work is to synthesize a zeolite-based catalystw ith ah ollow morphology and highly dispersed metal nanoparticles (NPs) encapsulated inside the zeolitem icropores.F or this purpose,w eh ave studied at reatment using tetraalkylammonium (TAA) bromides for the selective removal of al arge Pt particlef rom the outer surface of ah ollow Beta zeolite. TEM analysis reveals that we succeeded in the synthesis of ah ollow beta zeolite single crystal with encapsulatedp articles, with a high dispersion of 50-60%.T he molecular-sieve-type mechanism of the obtained catalystsw as evaluated in the model reactiono ft oluene and mesitylene catalytic hydrogenation. Thanks to the high dispersion. a1 0-fold activity enhancementh as been obtainedw ith respect to hollow beta zeolitesw ith encapsulated NPs recently described in the literature.Encapsulation of metal nanoparticles (NPs) within zeolite micropores provides particular selectivity that cannot be expected when NPs are supported on the external surface of the crystal, because the reactants can directly access the metal particles. One of the challenges is to prevent the formationo f metal particles at the outer surface of zeolite crystals, especially upon calcination andr eduction of the catalysts. [1] On the other hand, mass transport limitations might be expected when molecules diffuse through the molecular-sized pores to reach the encapsulated NPs, particularly when NPs are within large zeolite crystals. [2] We ando thers have recently reported the use and synthesis of hollow zeolite crystals, [3][4][5][6][7][8][9][10][11] as thin zeolite walls decrease the average diffusion length when compared to bulk zeolites, and thus shorten transport time. In the particular case of Pt NPs, encapsulatedi nh ollow Yz eolite single crystals, [12] the effectiveness factor of the zeolite,d efined as the fraction of the crystals effectively involved in the reaction, increased from approximately 65 %i nb ulk crystals to 98 %f or hollow crystalsf or the hydrogenation of cyclohexene.In other words, the use of hollow crystals enabled ah igh activity to be obtained while saving more than 35 wt %o fP tw ith respecttoabulk Yz eolite.One perspective for the enhancement of catalytic activity while providing am olecular-sieving type selectivity is the design of an "ideal" catalyst, which would correspondt o1 )a high metal loading (Pt > 1wt%)w ithout NPs at the outer surface, 2) ah igh metal dispersion (D > 40 %), and 3) short critical length (wall thickness < 150-200 nm; [12] Figure 1).The encapsulation of metal precursors into microporous materials is not easily achieved butm ethods based on ion exchange have been shown to be successful at relativelyh igh loading. [14][15][16] Encapsulation of Pt NPs in hollow beta single crystalsw as already achievedb yp re-impregnation [13] leading to the formation of rather large Pt particles (between 10 to 50 nm) with very poor dispersion ( % 3%). Despite ar educed diffusion length, such low metal dispersion did not lead to high catalytic act...