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Structural Analysis. Impact of the filler fraction in NCs. G. Baeza et al. Macromolecules 2013 Multi-scale filler structure in simplified industrial nanocomposite systems silica/SBR studied by SAXS and TEM. Multiscale Structure. network. aggregates. beads. R bead 10 nm. q -2.4.

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Presentation Transcript
slide1

Structural Analysis

  • Impact of the filler fraction in NCs

G. Baeza et al. Macromolecules 2013

Multi-scale filler structure in simplified industrial nanocomposite

systems silica/SBR studied by SAXS and TEM

slide2

Multiscale Structure

network

aggregates

beads

Rbead10 nm

q-2.4

Artistview

Tridimensionnal network built up from aggregates made of nanoparticles

Ragg40 nm

dbranch120 nm

  • si (Quantitative Model)
  • Densification of the silica network
  • Aggregates remain similar
slide3

Global View: 3-level Organization

analysis

network

aggregate

bead

High-q :

Bead form factor

qsi Rsi (R0= 8.55 nm  = 27%)

Medium-q :

qagg Ragg (35 – 40 nm) Interactions Between Aggregates

Low-q :

qbranch Network branches (lateral dimension  150 nm),

compatible with fractal aggregates (d2.4).

The network becomes denser and denser with si

Artist view:

network built up from Aggregates made of nanoparticles

slide4

Quantitative analysis: Aggregate Radius

Subtraction of the fractal law

Kratky Plots allow to extract <Ragg>

qagg

d  2.4

si

qagg

Morphology of an aggregate

Ragg Distribution Hypothesis

Ragg

slide5

Quantitative model

Scattering law linking structure and form (polydisperse case)

1) Determination of <Pagg>

Ragg distribution

Nagg distribution

Working hypothesis

*

Calculation

*Oberdisse, J.; Deme, B. Macromolecules 2002, 35 (11), 4397-4405

slide6

Quantitative model

Scattering law linking structure and form (polydisperse case)

Sapp (q) depends on local si in the branches = agg

inter

app

2) Determination of Sinter(q)

  • Estimation of agg: TEM

Same Working hypothesis

fract

  • Monte Carlo Simulation of polydisperse aggregates

Hard-SpherePotential (PY like)

agg

Semi-Empiriclaw from simulation

slide7

Self Consistent Model

  • Final determination of 

I(q) is read

Experimental

I(q) = f()

saxs

Results:

<Ragg> decreases slightly

 increases slightly

<Nagg>  constant !