Simultaneous time resolved SAXS and WAXS experiments using synchrotron radiation

Bras, Wim; Derbyshire, G.E.; Ryan, Anthony J.; Mant, G.; Felton, Anne; Lewis, Robert A.; Hall, Chris; Greaves, G.N.

doi:10.1016/0168-9002(93)90863-d

Cited by 169 publications

(107 citation statements)

References 10 publications

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“…tion Source (SRS), Daresbury (UK) [15]. The scattered X-ray intensities were recorded using a quadrant detector.…”

Section: Binary Sol Synthesismentioning

confidence: 99%

“…A strong increase of separation factors, which are mainly governed by Knudsen diffusion for mesoporous membranes (O~idea 1 ~ (MA/MB)I/2), tO molecular sieve-like separation factors, have been reported [2][3][4][5][6][7]. Non-Crystalline Solids 191 (1995) [1][2][3][4][5][6][7][8][9][10][11][12][13][14][15][16] ture of the polymeric sols. Also the structural evolution of sols as function of sol age is followed.…”

Section: Introductionmentioning

confidence: 99%

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Polymeric-silica-based sols for membrane modification applications: sol-gel synthesis and characterization with SAXS

Lange

Hekkink

Keizer

et al. 1995

Journal of Non-Crystalline Solids

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Polymeric SiO 2 and binary SiO2/TiO a, SiO2/ZrO 2 and SiO2/A120 3 sols, for ceramic membrane modification applications, have been prepared by acid-catalyzed hydrolysis and condensation of alkoxides in alcohol. The sols were characterized with small angle X-ray scattering, using synchrotron radiation. Directly after synthesis, the sols were found to consist of weakly branched polymeric structures with typical fractal dimensions of around 1.5 and radii of gyration of = 2 nm. The aggregation for silica sols obeys the tip-to-tip cluster-cluster aggregation model in the initial stages. Prehydrolysis of TEOS was found to be the best method to synthesize polymeric binary systems. Based on an analysis of film formation from sols consisting of weakly branched polymers, it is expected that consolidation of these polymers will result in microporous materials.

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“…tion Source (SRS), Daresbury (UK) [15]. The scattered X-ray intensities were recorded using a quadrant detector.…”

Section: Binary Sol Synthesismentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Polymeric-silica-based sols for membrane modification applications: sol-gel synthesis and characterization with SAXS

Lange

Hekkink

Keizer

et al. 1995

Journal of Non-Crystalline Solids

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“…Despite the scientific significance of the study of the effect of different processing conditions on the final product structure, it is more relevant for polymer industries to understand the structure development during polymer processing and in situ experiments are required. Attempts to perform online polymer processing experiments using synchrotron-based X-ray scattering experiments have already been conducted in the past two decades and ranged from simple crystallization experiments using differential scanning calorimetry (Bras et al, 1995) in combination with dedicated small/wide-angle X-ray scattering (SAXS/WAXS) beamlines (Bras et al, 1993), to more complicated experiments where fiber spinning (Terrill et al, 1998;Kolb et al, 2000) or even reactive processing was used (Elwell et al, 1994). However, previous SAXS/WAXS experiments have been limited to experimental protocols far from the industrial processing conditions as a result of the instrumental limitations.…”

Section: Introductionmentioning

confidence: 99%

Polymer crystallization studies under processing-relevant conditions at the SAXS/WAXS DUBBLE beamline at the ESRF

et al. 2013

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Recent developments on the experimental infrastructure and the acquisition of new detectors on the Dutch-Belgian beamline BM26B at the ESRF offer novel and promising possibilities for synchrotron X-ray experiments in the field of polymer crystallization under processing-relevant conditions. In this contribution, some of the most recent experiments mimicking conditions similar to those relevant for the plastics processing industry are discussed. Simultaneous thermal analysis and wide-angle X-ray scattering (WAXS) experiments, at the millisecond time-frame level, on -nucleated isotactic polypropylene (i-PP) samples subjected to ballistic cooling up to 230 K s À1 , show that the efficiency of the nucleating agent can be suppressed when quenched cooling rates higher than 130 K s À1 are used. In situ WAXS experiments using small-scale industrial equipment during a real film blowing process reveal the dependence of the onset of crystallinity (the so-called freeze line) and the crystal orientation as a function of different take-up and blow-up ratios. In situ small-angle X-ray scattering (SAXS) experiments during high-flow fields reveal the formation of shish and kebab structures in i-PP as a function of the imposed stress. Quantitative analysis of i-PP flow-induced structures is presented. The beamline specifications required to obtain high quality and industrially relevant results are also briefly reported.

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“…Combining SAXS with WAXS at synchrotron radiation sources (Bras et al 1993) has enabled these different regions of wavevector Q to be accurately measured with exposure times from 10 ms to minutes (Bras et al 2003). Q = 4π sin θ/λ, where 2θ is the scattering angle and λ the X-ray wavelength.…”

Section: Small-and Wide-angle Scatteringmentioning

confidence: 99%

Polyamorphism and the universal liquid–liquid critical point in the supercooled state

Greaves

2010

DLS Proc.

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The physics of critical phenomena is well established in systems as diverse as molecular fluids, crystalline alloys and magnetic materials. As the critical point is approached, the susceptibility increases anomalously and fluctuations give rise to dramatic opalescence. Evidence has recently emerged for the existence of a second critical point in the liquid state at supercooled temperatures, below which polyamorphic phases coexist differing in density but sharing the same composition. Whilst much attention has been paid to supercooled water, polyamorphic phases have been observed in many elemental and oxide liquids potentially offering routes to low-entropy glasses. Our recent direct observation of a polyamorphic phase transition in levitated molten yttria-alumina offers the first opportunity to study the associated critical point in a real supercooled system. In situ small-angle X-ray scattering records sharp rises in the average correlation length of density fluctuations and in the compressibility as the transition is approached. Both increases approximate to the universal power-law relations predicted by the three-dimensional Ising model in common with all critical point phenomena. The observation brings the second critical point predicted in liquids into line with other critical phenomena.

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Simultaneous time resolved SAXS and WAXS experiments using synchrotron radiation

Cited by 169 publications

References 10 publications

Polymeric-silica-based sols for membrane modification applications: sol-gel synthesis and characterization with SAXS

Polymeric-silica-based sols for membrane modification applications: sol-gel synthesis and characterization with SAXS

Polymer crystallization studies under processing-relevant conditions at the SAXS/WAXS DUBBLE beamline at the ESRF

Polyamorphism and the universal liquid–liquid critical point in the supercooled state

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