Topologically Ordered Amorphous Silica Obtained from the Collapsed Siliceous Zeolite, Silicalite-1-F: A Step toward “Perfect” Glasses

Haines, J.; Levelut, Claire; Isambert, Aude; Hébert, Philippe; Kohara, Shinji; Keen, David A.; Hammouda, Tahar; Andrault, Denis

doi:10.1021/ja904054v

Cited by 92 publications

(144 citation statements)

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“…Thus, our findings highlight the role of in situ and real-time PXRD monitoring as a complement to other experimental and computational studies of the structural landscape of metal-organic frameworks 40,41 . We note that the use of in situ monitoring to detect new phases appearing during milling may not be limited to metal-organic frameworks, but could very likely impact the understanding of structural transformations in related inorganic materials, such as zeolites and silicates, during mechanical processing or geological transformations 42 .…”

Section: Discussionmentioning

confidence: 99%

In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

et al. 2015

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Chemical and physical transformations by milling are attracting enormous interest for their ability to access new materials and clean reactivity, and are central to a number of core industries, from mineral processing to pharmaceutical manufacturing. While continuous mechanical stress during milling is thought to create an environment supporting nonconventional reactivity and exotic intermediates, such speculations have remained without proof. Here we use in situ, real-time powder X-ray diffraction monitoring to discover and capture a metastable, novel-topology intermediate of a mechanochemical transformation. Monitoring the mechanochemical synthesis of an archetypal metal-organic framework ZIF-8 by in situ powder X-ray diffraction reveals unexpected amorphization, and on further milling recrystallization into a non-porous material via a metastable intermediate based on a previously unreported topology, herein named katsenite (kat). The discovery of this phase and topology provides direct evidence that milling transformations can involve short-lived, structurally unusual phases not yet accessed by conventional chemistry.

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Section: Discussionmentioning

confidence: 99%

In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

et al. 2015

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“…The mechanical properties of PESIL were determined by measuring the XRD patterns as a function of pressure at room temperature on the polycrystalline sample. The equation of state (EOS) was obtained along with a test of resistance against pressure-induced amorphization 25 (Fig. 4).…”

Section: Synthesis Of Pesilmentioning

confidence: 99%

“…Silicalite is characterized by a framework of 4-, 5-, 6-and 10-membered rings of cornersharing SiO 4 tetrahedra forming interconnected, mutually orthogonal straight and sinusoidal 5.5 Å diameter channels (see ref. 25 and references therein). Silicalite can easily adsorb simple molecules, such as Ar, CO 2 refs 26-28), and straight n-alkanes (up to n ¼ 10), and, interestingly, computer simulations indicate that n-alkane chains easily adapt to the channels 29,30 .…”

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High-pressure synthesis of a polyethylene/zeolite nano-composite material

et al. 2013

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Meso/micro-porous solids, such as zeolites, are complex materials used in an impressive range of applications. Here we photo-polymerized ethylene using non-catalytic high-pressure techniques at 0.5-1.5 GPa under ultraviolet (351-364 nm) irradiation on a sub-nanometre scale in the channels of a pure SiO 2 zeolite, silicalite, to obtain a unique nano-composite material with drastically modified mechanical properties. The structure obtained contains single polyethylene chains, which adapt very well to the confining channels as shown by optical spectroscopy and X-ray diffraction. The formation of this nano-composite results in significant increases in bulk modulus and density, and the thermal expansion coefficient changes sign from negative to positive with respect to silicalite. Mechanical properties may thus be tuned by varying the amount of polymerized ethylene. Our findings could allow the high-pressure, catalyst-free synthesis of a unique generation of technological, functional materials based on simple hydrocarbons polymerized in confining meso/micro-porous solids.

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“…At ambient conditions, silicalite is characterized by a framework of four-, five-, six-, and ten-membered rings of SiO 4 tetrahedra with 5.5-Å pores (15) (Fig. 1, Left Inset).…”

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Silicon carbonate phase formed from carbon dioxide and silica under pressure

Santoro

Gorelli

Haines

et al. 2011

Proc. Natl. Acad. Sci. U.S.A.

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The discovery of nonmolecular carbon dioxide under high-pressure conditions shows that there are remarkable analogies between this important substance and other group IV oxides. A natural and long-standing question is whether compounds between CO 2 and SiO 2 are possible. Under ambient conditions, CO 2 and SiO 2 are thermodynamically stable and do not react with each other. We show that reactions occur at high pressures indicating that silica can behave in a manner similar to ionic metal oxides that form carbonates at room pressure. A silicon carbonate phase was synthesized by reacting silicalite, a microporous SiO 2 zeolite, and molecular CO 2 that fills the pores, in diamond anvil cells at 18-26 GPa and 600-980 K; the compound was then temperature quenched. The material was characterized by Raman and IR spectroscopy, and synchrotron X-ray diffraction. The experiments reveal unique oxide chemistry at high pressures and the potential for synthesis of a class of previously uncharacterized materials. There are also potential implications for CO 2 segregation in planetary interiors and for CO 2 storage.high-pressure chemistry | material science | optical spectroscopy C arbon dioxide and silicon dioxide are two archetypal, group IV oxides of paramount importance for fundamental and applied chemistry and planetary sciences. CO 2 is the dominant component of the atmosphere of Earth-like planets, exists in icy forms in outer planets and asteroids, plays an important role in volcanic and seismic processes, is used as a supercritical solvent for chemical reactions, and its anthropogenic production is a major environmental issue. SiO 2 is also one of the most abundant components of terrestrial planets, and an important technological material. The chemical relationship between CO 2 and SiO 2 , in particular their reactivity, is thus of interest. Although the two systems are both group IV oxides, they are remarkably different under ambient conditions, because CO 2 is molecular and is held together by C═O double bonds, whereas SiO 2 forms network structures involving single Si─O bonds. These bonding patterns radically change under pressure. Two nonmolecular CO 2 crystalline phases and a glassy form have been discovered above 30 GPa that bear similarities to SiO 2 (1-14). The crystalline phases contain carbon in fourfold coordination by oxygen (1-10, 13, 14), and mixtures of CO 4 and CO 3 units have been found in a glassy form that has been named carbonia (13).A possible approach to favor the chemical reaction between CO 2 and SiO 2 is to select a microporous silica polymorph, such as silicalite. At ambient conditions, silicalite is characterized by a framework of four-, five-, six-, and ten-membered rings of SiO 4 tetrahedra with 5.5-Å pores (15) (Fig. 1, Left Inset). Recently, it has been found that the pores can be completely filled by simple molecules such as CO 2 and Ar under pressure, which prevents pressure-induced amorphization (PIA) and stabilizes the crystalline framework up to at least 25 GPa at room temperature (1...

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Topologically Ordered Amorphous Silica Obtained from the Collapsed Siliceous Zeolite, Silicalite-1-F: A Step toward “Perfect” Glasses

Cited by 92 publications

References 50 publications

In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

In situ X-ray diffraction monitoring of a mechanochemical reaction reveals a unique topology metal-organic framework

High-pressure synthesis of a polyethylene/zeolite nano-composite material

Silicon carbonate phase formed from carbon dioxide and silica under pressure

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