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Reaction-induced phase separation in modified thermosetting polymers

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Book cover Polymer Analysis Polymer Physics

Part of the book series: Advances in Polymer Science ((POLYMER,volume 128))

Abstract

Thermosetting polymers are frequently used in formulations, including rubbers, thermoplastic polymers or oils, etc, in an amount of the order of 2–50 wt% with respect to the thermoset. This extra component, called the modifier, may initially be immiscible or may phase-separate during cure. This last process, i.e the reaction-induced phase separation, is the subject of this review. A thermodynamic description of the process is made, using the Flory-Huggins equation at two approximation levels, i.e. a quasi-binary approach and a multicomponent treatment taking polydispersity of constituents into account. Thermodynamic factors affecting the phase separation process are thus established. Nucleation and growth (NG) and spinodal demixing (SD) are considered as possible phase separation mechanisms. Factors promoting one or the other process are discussed. The control of morphologies generated is analyzed on the basis of thermodynamic and kinetic arguments. Ideas for obtaining particular morphologies enhancing particular properties are put forward.

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Abbreviations

a:

parameter included in the relationship between the Flory-Huggins interaction parameter and the absolute temperature

A4 :

tetrafunctional monomer

b:

slope of the relationship between the Flory-Huggins interaction parameter and the inverse of absolute temperature

b1, b2 :

constants included in the dependence of x with temperature and composition

B2 :

difunctional monomer

Cpart :

concentration of dispersed phase particles

\(\bar D\) :

average diameter of dispersed phase particles

d0, d1, d2 :

constants included in the dependence of x with temperature and composition

E:

elastic (Young's) modulus

Em,n :

oligomer produced by polycondensation, containing n molecular units of monomer and m molecular units of comonomer (hardener)

g:

interaction parameter depending on both temperature and composition

G:

Gibbs free energy

g0, g1, g10, g11 :

constants included in the dependence of g with temperature and composition

GIc :

fracture energy

h:

parameter in the Schultz-Zimm equation

H:

enthalpy

II :

integrated intensity of the scattered light

I(q) :

intensity of the scattered light as a function of the scattering vector

K:

ratio of the phase separation rate with respect to the cure reaction rate

kB :

Boltzmann constant

KIc :

critical stress intensity factor

M:

modifier

\(\bar M\) i :

molar mass of component i

\(\bar M\) n :

number-average molar mass

N:

number of moles

p:

conversion

P:

average species of the polymer

Pi :

macromolecule containing i monomer units

Pi,j,k :

macromolecule obtained by chain polymerization, containing i monomer units, j functional groups and k active centres

q:

scattering vector

r:

ratio of amine to epoxy equivalents

R:

gas constant

S:

entropy

t:

time

T:

absolute temperature

Tg :

glass transition temperature

gelTg:

temperature where gelation and vitrification take plase simultaneously

Tg∞ :

ultimate glass transition temperature of the polymer network

Tr :

reaction temperature

U:

parameter in the Schulz-Zimm equation

V:

molar volume

v0 :

initial reaction rate

VD :

volume fraction of dispersed phase

VMS :

molar volume of the unit segment of a polymeric modifier

VPS :

molar volume of the unit segment of the thermosetting polymer

Vr :

molar volume of the unit cell (reference volume)

VT :

total volume of the system (extensive property)

x:

denotes the x-mer of a polymeric modifier

\(\overline {X_n }\) :

number-average degree of polymerization

\(\overline {X_w }\) :

mass-average degree of polymerization

y:

denotes the y-mer of the thermosetting polymer

Zc :

coordination number of a unit cell

Zi :

ratio of the molar volume of component i with respect to the molar volume of the unit cell

α-phase:

thermoset-rich phase

αi :

thermal expansion coefficient of component i

β-phase:

modifier-rich phase produced in the course of the primary phase separation

x:

Flory-Huggins interaction parameter

δ:

solubility parameter

δ-phase:

modifier-rich phase inside particles of the β-phase (secondary phase separation)

ΔG:

Gibbs free energy of mixing per unit volume of system

ΔGc :

free energy barrier for nucleation

ΔGM :

Gibbs free energy of mixing (extensive property)

ΔH:

enthalpy of mixing per unit volume of system

ΔHM :

enthalpy of mixing (extensive property)

ΔS:

entropy of mixing per unit volume of system

ΔSM :

entropy of mixing (extensive property)

Δμi :

chemical potential of component i

ε′:

exchange energy

εij :

energy of a contact between components i and j

φ:

volume fraction

γ:

constant included in the dependence of γ with temperature and composition

γ-phase:

thermoset-rich phase inside particles of the β-phase (secondary phase separation)

Γ:

gamma function

η:

viscosity

Λ:

interaction parameter with units of energy per unit volume

σ0 :

interfacial tension

σy :

yield stress

ω:

mass fraction

CP:

value of the cloud point

crit:

value at the critical point

gel:

value at the gel point

M:

modifier

0:

initial value

P:

polymer

S:

silicon chip

x:

x-mer of a polymeric modifier

y:

y-mer of the thermosetting polymer

AN:

acrylonitrile

ATBN:

amino-terminated butadiene-acrylonitrile copolymer

BD:

butadiene

BMC:

bulk moulding compound

CE:

cyanate ester

CO:

castor oil

CP:

cloud point

CPC:

cloud-point curve

CS:

core-shell particles

CTBN:

carboxyl-terminated butadiene-acrylonitrile copolymer

3DCM:

4,4′-diamino-3,3′-dimethyldicyclohexyl-methane

DGEBA:

diglycidyl ether of bisphenol A

EDA:

ethylenediamine

ETBN:

epoxy-terminated butadiene-acrylonitrile copolymer

FH:

Flory-Huggins

GMA:

glycidyl methacrylate

HIPS:

high-impact polystyrene

IPN:

interpenetrated polymer network

LCST:

lower-critical-solution temperature

LS:

light scattering

LT:

light transmission

NFBN:

non-functionalized copolymer of butadiene and acrylonitrile

NG:

nucleation-growth

NR:

nucleation rate

PDLC:

polymer-dispersed liquid crystal

PE:

polyester

PEI:

poly(etherimide)

PES:

poly(ethersulfone)

PICS:

pulse-induced-critical scattering

PVAc:

poly(vinylacetate)

PVME:

poly(vinylmethylether)

R:

rubber

S:

spinodal curve

SAXS:

small-angle-X-ray scattering

SBR:

styrene butadiene random copolymer

SD:

spinodal demixing

SEM:

scanning electron microscopy

SMC:

sheet moulding compound

SZ:

Schulz-Zimm equation

TEM:

transmission electron microscopy

TP:

thermoplastic

TTT:

time-temperature-transformation diagram

UCST:

upper-critical-solution temperature

UP:

unsaturated polyester

UV:

ultraviolet light

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Authors and Affiliations

  1. Institute of Materials Science and Technology (INTEMA), University of Mar del Plata and National Research Council (CONICET), J.B. Justo 4302, 7600, Mar del Plata, Argentine

    Roberto J. J. Williams

  2. Institute of Chemical Physics in Chernogolovka Russian Academy of Sciences, 142432, Chernogolovka, Moscow region, Russia

    Boris A. Rozenberg

  3. Laboratoire des Matériaux Macromoléculaires, URA CNRS No. 507, Institut National des Sciences Appliquées de Lyon, 20, Avenue A. Einstein, 69621, Villeurbanne Cedex, France

    Jean-Pierre Pascault

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Williams, R.J.J., Rozenberg, B.A., Pascault, JP. (1997). Reaction-induced phase separation in modified thermosetting polymers. In: Polymer Analysis Polymer Physics. Advances in Polymer Science, vol 128. Springer, Berlin, Heidelberg. https://doi.org/10.1007/3-540-61218-1_7

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  • DOI: https://doi.org/10.1007/3-540-61218-1_7

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