Monitoring the structure of water soluble silicates

Halász, I.; Agarwal, Mukesh; Li, Runbo; Miller, N.H.

doi:10.1016/j.cattod.2006.09.032

Cited by 28 publications

(12 citation statements)

References 84 publications

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“…We report here that 0.2-3 mol/L aqueous solutions of crystalline sodium metasilicate, Na 2 SiO 3 , contain almost exclusively monosilicate ions at pH > 10 unlike most other aqueous sodium silicate solutions typically manufactured from amorphous glasses [43]. Thus, these metasilicate solutions are excellent models for studying the IR and Raman spectra of sodium silicate monomers.…”

Section: Introductionmentioning

confidence: 94%

“…However, only a small group from these authors has assigned certain vibrational bands to specific molecular structures like monomers or siloxane chains, rings, etc. [16][17][18][19][20]26,35,38,41] and even these contain much inconsistency [42][43][44][45][46]. One impediment to more reliable structural interpretations is the lack of relevant model compounds.…”

Section: Introductionmentioning

confidence: 99%

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Vibrational spectra and dissociation of aqueous Na2SiO3 solutions

Halász¹,

Agarwal²,

Li³

et al. 2007

Catal Lett

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To facilitate molecular spectroscopic observation of the mysterious transition of dissolved sodium silicate molecules into nanoparticles of desired silica gel and zeolite structures, the IR and Raman spectra of Na 2 H 2 SiO 4 monomers are studied here in details. It is demonstrated that the 3-0.2 mol/L aqueous solutions of Na 2 SiO 3 and Na 2 SiO 3 Â 9H 2 O contain mostly Na 2 H 2 SiO 4 monomers dissociated about 30%-80%, respectively. In contrast to the common belief the Si-O vibrations of these monomers depend on their dissociation level generating FTIR and Raman bands which are frequently associated with polymer silica structures in the current literature. To stay consistent with the molweight and dissociation measurements, these vibrational assignments are revised in this paper. Some unique and unexpected effects of D 2 O used instead of H 2 O as solvent are also reported.

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Section: Introductionmentioning

confidence: 94%

Section: Introductionmentioning

confidence: 99%

Vibrational spectra and dissociation of aqueous Na2SiO3 solutions

Halász¹,

Agarwal²,

Li³

et al. 2007

Catal Lett

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“…The structure of silicate species dissolved in aqueous media is accessible with Raman spectroscopy. 56 The Si-O vibration related Raman spectra of silicates are usually better resolved than the corresponding IR spectra. Raman is convenient for characterizing the O-Si-O bending vibrations of various siloxane ring systems at wavenumbers below 400 cm À1 which are not accessible by the common mid-IR spectrometers.…”

Section: Raman Spectroscopymentioning

confidence: 99%

Methods for in situ spectroscopic probing of the synthesis of a zeolite

2010

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Unraveling the crystallization mechanism of zeolites remains an increasingly important challenge in chemistry. During the last decade, in situ spectroscopic methods have provided an unprecedented level of detail of the underlying molecular mechanisms and their kinetics. Magnetic resonance, vibrational and X-ray absorption techniques have emerged as principal tools for the in situ observation of crystallization. In this tutorial review, we discuss how these in situ methods have contributed to our understanding of the complex and diverse molecular processes that govern zeolite crystallization.

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“…The transition from a highly connected tetrahedral structure (such as quartz and amorphous silica) to a weakly or un-connected tetrahedral units (such as CaSiO 3 wollastonites or lead-based glaze) as caused by the addition of fluxing agents is reflected in the Raman spectrum by modifications of the intensity of the Si-O stretching multiplet (centre of gravity ~950 to 1150 cm -1 ) vs. the bending one (centre of gravity ~500 to 600 cm -1 ) [88]. The relationship between the Raman index of polymerisation (Ip = A 500 /A 1000 with A being the area under the Raman band), the glass composition and the processing temperature is now well documented [28,37,88,89,92,96,[123][124][125][126][127]. For instance this has been used to classify silver-containing yellow stained glass replicas [28] and ancient red or yellow stained glasses [96,100]: for instance a clear relationship was established between the polymerization index, the Area of Q n components and the b* colour coordinate as a function of the silver content and its degree of reduction [28].…”

Section: Non-destructive Analysesmentioning

confidence: 99%

The Use of Metal Nanoparticles to Produce Yellow, Red and Iridescent Colour, from Bronze Age to Present Times in Lustre Pottery and Glass: Solid State Chemistry, Spectroscopy and Nanostructure

Colomban

2009

JNanoR

154

128

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Abstract. The use of metal nanoparticles dispersed in an optically clear matrix by potters and glassmakers from the Bronze Age up to the present time is reviewed from the solid state chemistry and material science point of view. The nature of metal (gold, silver or copper), the importance of some other elements (Fe, Sn, Sb, Bi) added to control metal reduction in the glass in relation to the firing atmosphere (combined reducing oxidizing sequences, role of hydrogen and water) are considered in the light of ancient Treatises and recent analyses using advanced techniques (FIB-TEM, EXAFS,…) and classical methods (optical microscopy, UV-visible absorption). The different types of colour production, by absorption/reflection (red, yellow) or diffraction (iridescence) and the relationship between nanostructure (metal particle dispersion, layer stacking) and lustre colour are discussed. The very specific interaction between light and the metal nanoparticle makes Raman scattering a very useful "bottom up" technique to study the local glass structure around the metal particles as well as to detect incomplete metal reduction or residues tracing the preparation route, hence making it possible to differentiate between genuine artefacts and fakes.

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Monitoring the structure of water soluble silicates

Cited by 28 publications

References 84 publications

Vibrational spectra and dissociation of aqueous Na2SiO3 solutions

Vibrational spectra and dissociation of aqueous Na2SiO3 solutions

Methods for in situ spectroscopic probing of the synthesis of a zeolite

The Use of Metal Nanoparticles to Produce Yellow, Red and Iridescent Colour, from Bronze Age to Present Times in Lustre Pottery and Glass: Solid State Chemistry, Spectroscopy and Nanostructure

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