Synthesis and characterization of siloxane-titania materials

Dirè, Sandra; Babonneau, Florence; Carturan, G.; Livage, Jacques

doi:10.1016/s0022-3093(05)80594-0

Cited by 40 publications

(26 citation statements)

References 7 publications

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“…Besides several workers, especially Sanchez and Babonneau, have shown that in gels and xerogels containing both silicon and titanium, there was an initial formation of Ti-O-Si bonds, which were not stable and tend to disappear in the course of several hours [15,[22][23][24]27]. However, this was only proved on aged gels upon long waiting times, and in addition with a relatively high titanium proportion.…”

Section: Resultsmentioning

confidence: 99%

“…Despite their apparent similarity, the two transition metal alcoxides lead to final materials with relatively different structures, which have been studied by several techniques, including infrared spectroscopy [13][14][15][16][17][18][19][20][21], Raman [20], X ray scattering [14,16,17,[21][22][23][24], NMR [13][14][15][16][21][22][23][24][25][26][27][28][29][30], electron microscopy, etc. .…”

Section: Introductionmentioning

confidence: 99%

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Analysis of the gelation process of hybrid silica–zirconia and silica–titania gels using two different grafted electroactive probes

Audebert¹,

Miomandre²,

Sadki³

et al. 2006

Journal of Electroanalytical Chemistry

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Analysis of the gelation process of hybrid silica–zirconia and silica–titania gels using two different grafted electroactive probes

Audebert¹,

Miomandre²,

Sadki³

et al. 2006

Journal of Electroanalytical Chemistry

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“…This catalytic effect of metal alkoxides can prevent the formation of volatile low molecular weight species such as short-chain oligomers and cyclic siloxanes during the condensation reactions. [15,16] Figure 1 is a depiction of the interconnecting network formed between the cured polysiloxane and the metal-oxoclusters.…”

Section: Introductionmentioning

confidence: 99%

Effect of Mixed Sol‐Gel Precursors on the Metal‐Oxo Phase Within a UV‐Curable Silicone Hybrid Material

Dworak

Soucek

2006

Macro Chemistry & Physics

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Summary: An inorganic hybrid material was produced using a polysiloxane binder and metal‐oxo‐clusters which were derived from sol‐gel precursors. The continuous phase is composed of an elastomeric polysiloxane functionalized with cycloaliphatic epoxide groups. Pendant alkoxy silane groups serve as a coupling agent to form a network between the metal‐oxo‐clusters and the crosslinked polysiloxane. Methyl, cyclopentyl, and cyclohexyl substituted polysiloxanes were formulated with a variety of sol‐gel precursors (tetraethylorthosilicate oligomers, titanium(IV) iso‐propoxide, zirconium(IV) propoxide, and zinc acetate). Phase‐modulated FT‐IR, X‐ray photoelectron spectroscopy, solid state 29Si NMR, and solid state 13C NMR were used to investigate the internal structure of the mixed metal‐oxo/silicon‐oxo colloids prepared within the cured polysiloxane matrix. Results indicate that the cycloaliphatic groups inhibit the complete hydrolysis and condensation of the pendant triethoxysilane group and reaction of the sol‐gel precursors. Analysis also indicated that the metal‐oxo‐clusters were comprised of mixed species of sol‐gel precursors resulting in hetero‐bonded (SiOMetal) colloids.Possible network compositions of the cured material (a) specific metal‐oxo‐clusters, (b) hetero‐bonded metal‐oxo‐clusters, and (c) core/shell type metal‐oxo‐cluster configuration.magnified imagePossible network compositions of the cured material (a) specific metal‐oxo‐clusters, (b) hetero‐bonded metal‐oxo‐clusters, and (c) core/shell type metal‐oxo‐cluster configuration.

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“…Así las reacciones entre TEOS-PDMS o TEOS-DMDES (dimetil-dietoxisilano) y alcóxidos de titanio se ha estudiado con gran profundidad mediante 29 Si RMN (17). Por otro lado, la evolución estructural así como las propiedades de estos materiales se han seguido mediante 17 O RMN, 1 H RMN y espectroscopia de absorción de rayos X (6,12,(17)(18)(19). Sin embargo la espectroscopia infrarroja ha sido muy poco utilizada hasta la fecha.…”

Section: Introductionunclassified

Seguimiento por espectroscopia infrarroja (FT-IR) de la copolimerización de TEOS (tetraetilortosilicato) y PDMS (polidimetilsiloxano) en presencia de tbt (tetrabutiltitanio)

Téllez¹,

Rubio²,

Peña-Alonso³

et al. 2004

Bol. Soc. Esp. Ceram. Vidr.

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Se han preparado materiales híbridos por medio de reacciones de hidrólisis y condensación de alcóxidos de Si y Ti (TEOS y TBT, respectivamente) y de reacciones de copolimerización de éstos con polidimetilsiloxano (PDMS). Se han estudiado las citadas reacciones mediante espectroscopia FT-IR, desde el mismo comienzo hasta la obtención del material final. La hidrólisis del TEOS así como la autocondensación del os grupos Si-OH generados tanto para formar cadenas entrecruzadas como lineales se han seguido mediante las bandas situadas a 880, 1180 y 1150 cm -1 , respectivamente. La policondensación de dichos grupos con PDMS se ha seguido por la banda a 850 cm -1 . Por otro lado, la hidrólisis del TBT y la autocondensación de grupos Ti-OH se han seguido por la banda situada a 1130 y por la variación de la absorbancia en la región espectral 770-510 cm -1 , respectivamente. La formación de enlaces Si-O-Ti por condensación de grupos Si-OH y Ti-OH se ha seguido mediante la banda a 936 cm -1 . Los resultados obtenidos han mostrado que las reacciones de hidrólisis y policondensación dependen de la concentración de TBT en el medio de reacción. La formación de estructuras entrecruzadas de enlaces Si-O-Si se ve favorecida por el TBT, si bien por el contrario éste impide la reacción de copolimerización TEOS-PDMS. La autocondensación de grupos Si-OH y Ti-OH es muy rápida dando lugar a enlaces Si-O-Si y Ti-O-Ti, respectivamente. También se forman enlaces Si-O-Ti en los comienzos de la reacción, sin embargo éstos tienden a desaparecer en el transcurso de la misma. Finalmente se ha estudiado la variación de la concentración de cadenas cíclicas y lineales de PDMS durante toda la reacción. Palabras Clave: Ormosil, sol-gel, hidrólisis, condensación, FT-IR. FT-IR spectroscopy study of the reaction of obtention of hybrid materialsHybrid materials have been prepared in this work through the reactions of Si and Ti alkoxides (TEOS and TBT, respectively) and polydimethil siloxane (PDMS). These reactions have been studied by means of FT-IR spectroscopy during the whole reaction time. The hydrolysis of TEOS molecule has been followed by the 880 cm -1 band, and the self-condensation reactions through the 1180 and 1150 cm -1 bands. Polycondesation reaction between Si-OH groups and PDMS molecules has been followed by the 850 cm -1 band. On the other hand, the hydrolysis reaction of TBT and the self-condensation of Ti-OH groups have been followed by the 1130 and 770-510 cm -1 bands, respectively. Finally the condensation reaction between Si-OH and Ti-OH groups have been studied by the 936 cm -1 band. Results have shown that hydrolysis and condensation reactions are depending on TBT concentration. The formation of Si-O-Si cross-linked structures increases with the TBT concentrations in the reaction. The selfcondensation reaction of Si-OH grups or Ti-OH grous is very reapid forming Si-O-Si and Ti-O-Ti bonds, respectively. However, the Si-O-Ti bonds which are formed during the first moments of reaction are also rapidly broken due to H 2 O molecules or...

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Synthesis and characterization of siloxane-titania materials

Cited by 40 publications

References 7 publications

Analysis of the gelation process of hybrid silica–zirconia and silica–titania gels using two different grafted electroactive probes

Analysis of the gelation process of hybrid silica–zirconia and silica–titania gels using two different grafted electroactive probes

Effect of Mixed Sol‐Gel Precursors on the Metal‐Oxo Phase Within a UV‐Curable Silicone Hybrid Material

Seguimiento por espectroscopia infrarroja (FT-IR) de la copolimerización de TEOS (tetraetilortosilicato) y PDMS (polidimetilsiloxano) en presencia de tbt (tetrabutiltitanio)

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