The formation of zeolites from solution – Analysis by mass spectrometry

Lim, Ivy H.; Schräder, Wolfgang

doi:10.1016/j.micromeso.2012.04.059

Cited by 39 publications

(29 citation statements)

References 152 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Mass spectrometry (MS) allows the investigation of oligomeric species in prenucleating and nucleating silicate solutions . In contrast to NMR, MS is sensitive enough to monitor the evolution of individual silicate species as a function of aging time.…”

Section: Resultsmentioning

confidence: 99%

Zeolite Beta Formation from Clear Sols: Silicate Speciation, Particle Formation and Crystallization Monitored by Complementary Analysis Methods

Castro

Haouas

Lim

et al. 2016

Chemistry A European J

Self Cite

View full text Add to dashboard Cite

The formation of silicate nanoaggregates (NAs) at the very early stages of precursor sols and zeolite beta crystallization from silicate nanoparticles (NPs) are investigated in detail using a combination of different analysis methods, including liquid-state Si, Al, N, and H NMR spectroscopy, mass spectrometry (MS), small-angle X-ray scattering (SAXS), X-ray diffraction (XRD), and transmission electron microscopy at cryogenic temperatures (cryo-TEM). Prior to hydrothermal treatment, silicate NAs are observed if the Si/OH ratio in the reaction mixture is greater than 1. Condensation of oligomers within the NAs then generates NPs. Aluminum doped into the synthesis mixtures is located exclusively in the NPs, and is found exclusively in a state that is fourfold connected to silicate, favoring their condensation and aggregation. These results are in agreement with general trends observed for other systems. Silicate NAs are essential intermediates for zeolite formation and are generated by the aggregation of hydrated oligomers, aluminate, and templating cations. Subsequent further intra-nanoaggregate silicate condensation results in the formation of NPs. H and N liquid NMR as well as diffusion ordered spectroscopy (DOSY) experiments provide evidence for weakly restricted rotational and translational mobility of the organic template within NAs as a consequence of specific silicate-template interactions. NAs thus appear as key species in clear sols, and their presence in the precursor sol favors silicate condensation and further crystallization, promoted either by increasing the Si/OH ratio or by heating.

show abstract

Section: Resultsmentioning

confidence: 99%

Zeolite Beta Formation from Clear Sols: Silicate Speciation, Particle Formation and Crystallization Monitored by Complementary Analysis Methods

Castro

Haouas

Lim

et al. 2016

Chemistry A European J

Self Cite

View full text Add to dashboard Cite

show abstract

“…12 There are also a few examples highlighting the potential in using ESI-MS and cryospray (temperature controlled) electrospray mass spectrometry (CSI-MS) to investigate the self-assembly processes occurring during the formation of zeolites and MOFs. 11,[13][14][15][16][17][18][19] Herein, we investigate the well-known isostructural series CPO-27-M, also denoted M2(dhtp), M2(dobdc) (dhtp/dobdc 4-= C8H2O6 4-(2,5-dihydroxyterephthalate)) or M-MOF-74, where M = Co 20 and Ni. 21 The structure is also formed with other divalent cations such as M = Mg, 22 Mn, 23 Zn, 24 Fe, [25][26] Cu, [27][28][29] and Cd.…”

Section: Introductionmentioning

confidence: 99%

Electrospray Mass Spectrometry Investigation into the Formation of CPO-27

Rosnes

Mathieson

Törnroos

et al. 2019

Crystal Growth & Design

View full text Add to dashboard Cite

Electrospray ionisation mass spectrometry (ESI-MS) has been utilised to investigate the self-assembly processes occurring during the formation of the microporous metal-organic framework CPO-27-M (M = Co, Ni). The mono-and dinuclear building units {M(Hxdhtp)} and {M2(Hxdhtp)}, where Hxdhtp is the organic linker HxC8O6 and fragments thereof, were identified as key species present in the reaction mixture during the product formation. Time resolved powder X-ray diffraction analysis were used to follow the synthesis, and confirm that no other crystalline

show abstract

“…A simplified system based on templated pure silica precursor suspensions enabling the direct study of the molecular assembly process and formation of zeolite nanocrystals has been investigated in details by many groups. A recent review paper has summarized the main reports on the formation of zeolites from clear suspensions [4,29]. In general in pure silica precursor systems, the initial formation process involves the hydrolysis of alkoxysilanes followed by condensation-polymerization, and ultimately formation of discrete particles smaller than five nanometers.…”

Section: Views On Crystallization Mechanism Of Zeolitesmentioning

confidence: 99%

“…The approaches applied toward nanosized molecular sieves are (i) synthesis from clear precursor suspensions in the presence of organic template, (ii) low temperature synthesis from highly alkaline organic-template-free hydrogels, and (iii) alternative methods including ionothermal, seed-induced and confined space synthesis [29][30][31][32][33]. In general the subdivision of any material into fine particles leads to immense specific surface areas that affect their properties.…”

Section: Nanosized Zeolitesmentioning

confidence: 99%

Progress in zeolite synthesis promotes advanced applications

Zaarour

Dong

Naydenova³

et al. 2014

Microporous and Mesoporous Materials

160

View full text Add to dashboard Cite

a b s t r a c tThis article outlines the importance of zeolite synthesis and their unique physicochemical characteristics promoting advanced applications. The main strategies for preparation of zeolites including organic-template assisted, organic-template free and alternative procedures are considered for synthesis of crystallites offering control and fine-tuning of their properties. Besides, rational design of zeolites with pre-determined structure, porosity, size, morphology, and composition are more viable by studying carefully the chemical and physical parameters controlling the zeolite synthesis and understanding the crystallization mechanism. Finally, a particular attention to the preparation of zeolites with nanosized dimensions and their utilization in innovative applications including photovoltaic, medicine and holographic sensors are presented.

show abstract

The formation of zeolites from solution – Analysis by mass spectrometry

Cited by 39 publications

References 152 publications

Zeolite Beta Formation from Clear Sols: Silicate Speciation, Particle Formation and Crystallization Monitored by Complementary Analysis Methods

Zeolite Beta Formation from Clear Sols: Silicate Speciation, Particle Formation and Crystallization Monitored by Complementary Analysis Methods

Electrospray Mass Spectrometry Investigation into the Formation of CPO-27

Progress in zeolite synthesis promotes advanced applications

Contact Info

Product

Resources

About