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Crystallization, Micro- and Nano-structure, and Melting Behavior of Polymer Blends

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Abstract

When the melt of a crystalline polymer is cooled to a temperature between the glass transition and the equilibrium melting point, the thermodynamic requirement for crystallization is fulfilled.

In a crystallizable miscible blend, however, the presence of an amorphous component, either thermoplastic or thermosetting, can either increase or decrease the tendency to crystallize depending on the effect of the composition of the blend on its glass transition and on the equilibrium melting point of the crystallizable component and also on the curing extent and conditions in case of thermosetting amorphous component. The type of segregation of the amorphous component, influenced by parameters such as crystallization conditions, chain microstructure, molecular weight, blend composition, and curing extent, determines to a large extent the crystalline morphology of a crystallizable binary blend. Separate crystallization, concurrent crystallization, or cocrystallization can occur in a blend of two crystallizable components. The spherulite growth of the crystallizable component in miscible blends is influenced by the type and molecular weight of the amorphous component, the former affecting the intermolecular interactions between both components and the latter the diffusion of the amorphous component. The blend composition, the crystallization conditions, the degree of miscibility and the mobility of both blend components, and the nucleation activity of the amorphous component are important factors with respect to the crystallization kinetics. The melting behavior of crystallizable miscible blends often reveals multiple DSC endotherms, which can be ascribed to recrystallization, secondary crystallization, or liquid-liquid phase separation. Complex crystallization behavior develops in miscible blends containing a crystallizable thermoplastic and a curable thermosetting component. That depends on the temperature and time of curing the thermosetting and also on whether crystallization is initiated before, during, or after the curing process.

For the discussion of the crystallization and melting behavior in immiscible polymer blends, a division into three main classes is proposed.

In blends with a crystallizable matrix and an amorphous dispersed phase, both the nucleation behavior and the spherulite growth rate of the matrix can be affected. Nucleation of the matrix always remains heterogeneous; however, the amount of nuclei can be altered due to migration of heterogeneous nuclei during melt-mixing. Blending can also influence the spherulite growth rate of the matrix. During their growth, the spherulites can have to reject, occlude, or deform the dispersed droplets. In general, the major influence of blending is a change in the spherulite size and semicrystalline morphology of the matrix.

A completely different behavior is reported for blends in which the crystallizable phase is dispersed. Fractionated crystallization of the dispersed droplets, associated with different degrees of undercooling and types of nuclei, is the rule. The most important reason is a lack of primary heterogeneous nuclei within each crystallizable droplet. An important consequence of fractionated crystallization may be a drastic reduction in the degree of crystallinity.

When two crystallizable components are blended, a more complex behavior due to the influence of both phases on each other is expected. In general, the discussion for matrix crystallization and droplet crystallization can be combined. However, crystallization of one of the phases can sometimes directly induce crystallization in the second phase. As a consequence, the discussion of blends of this type has been subdivided with respect to the physical state of the second phase during crystallization. The special case of “coincident crystallization,” in which the two phases crystallize at the same time, is discussed. Finally, the effect of compatibilization of crystalline/crystalline polymer blends is briefly reviewed.

A new section has been added, introduced to deal with crystallization phenomena in immiscible polymer blends containing nanoparticles. Recent reports, although few, discuss the effect of nanoparticles on crystallization and melting in immiscible polymer blends.

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Dedication and Acknowledgments

Professor Emeritus Dr. Gabriël Groeninckx would like to dedicate this chapter to all his former master and Ph.D. students, postdocs, and colleagues of the Laboratory for Macromolecular Structure Chemistry of the Catholic University of Leuven (KU Leuven, Heverlee, Belgium) for their valuable contribution in the field of polymer blends and related domains. He also would like to fully express his acknowledgments to the KU Leuven where he spent his scientific career from 1965 to 2010. And last but not least, he also has the great pleasure of dedicating this chapter 5 to his wife Anne-Marie and his children Christine, Filip, and Mark but also to his grandchildren Maartje, Nikolaas, Lineke, Noortje, and Luca. Each of them made him very happy in their own way.

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Authors and Affiliations

  1. Department of Chemistry, Division of Molecular and Nanomaterials, Laboratory of Macromolecular Structure Chemistry, Catholic University of Leuven, Celestijnenlaan 200F, 3001, Heverlee, Belgium

    G. Groeninckx & V. Everaert

  2. Laboratoire de Chimie Appliquée (LAC) DGRSDT, Institut des Sciences et Technologies, Ctr Univ Ain Temouchent, Bp/284, Ain Temouchent, 46000, Algeria

    C. Harrats

  3. Textile Functionalisation & Surface Modification, R&D/CENTEXBEL, Technologiepark 7, Zwijnaarde, 9052, Algeria

    M. Vanneste

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  1. G. Groeninckx
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Correspondence to G. Groeninckx .

Editor information

Editors and Affiliations

  1. Industrial Materials Institute, National Research Council of Canada, Boucherville, Québec, Canada

    Leszek A. Utracki

  2. Department of Chemistry and Fire Retardant Research Facility, Marquette University, Milwaukee, Wisconsin, USA

    Charles A. Wilkie

Glossary

AN

Acrylonitrile

aPMMA

Atactic poly(methyl methacrylate)

aPS

Atactic polystyrene

BR

Butyl rubber

CPE

Chlorinated polyethylene

DDS

4,4′-diaminodiphenylsulfone

DGEBA

Diglycidyl ether of bisphenol A

DHDPE

Deuterated high-density polyethylene

EBA

Ethylene butylacrylate

EEA

Elastomeric copolymer from ethylene and ethyl acrylate

EGMA

Ethylene glycidyl methacrylate

EPDM

Elastomeric terpolymer from ethylene, propylene, and a non-conjugated diene

EPR

Elastomeric ethylene-propylene copolymer

EPR-g-SA

Elastomeric ethylene-propylene copolymer grafted with styrene acrylonitrile

ER

Epoxy resin

EVAc

Poly(ethylene-co-vinyl acetate) (random)

FVA

Poly(vinyl acetate-co-di-n-tetradecyl fumarate) (alternating)

GMA

Glycidyl methacrylate copolymer

HDPE

High-density polyethylene

iP(p-Me-S)

Isotactic copolymer of styrene and p-methyl styrene

iPEMA

Isotactic poly(ethyl methacrylate)

iPMMA

Isotactic poly(methyl methacrylate)

iPS

Isotactic polystyrene

LDPE

Low-density polyethylene

LLDPE

Linear low-density polyethylene

MA or MAH

Maleic anhydride

MCDEA

4,4′-methylenebis(3-chloro-2,6-diethylaniline

P(4-Me-pentene)

Poly(4-methyl pentene)

P(E)0.43(K)0.57

Random copolymer of phenyl ether and phenyl ketone

P(iPr-vinyl ether)

Poly(isopropyl-vinyl ether)

P(sec-But-vinyl ether)

Poly(sec-butyl vinyl ether)

PA-11

Polyamide 11

PA-12

Polyamide 12

PA-6

Polyamide 6

PA-66

Polyamide 66

PAr

Polyarylate

PBA

Poly(1,4.butylene adipate)

PBT

Polybutyleneterephthalate

PC

Bisphenol-A polycarbonate

PCDS

Poly(1,4-cyclohexane-dimethylene succinate)

PCL

Poly-e-caprolactone

PDPA

Poly(2,2-dimethyl-1,3-propylene adipate)

PDPS

Poly(2,2-dimethyl-1,3-propylene succinate)

PE

Polyethylene

PEA

Poly(ethylene adipate)

PECH

Poly(epichlorohydrin)

PED

n-Dodecyl ester terminated poly(ethylene glycol)

PEE

Poly(ester-ether) segmented block copolymers

PEEEK

Poly(ether ether ether ketone)

PEEK

Poly(ether ether ketone)

PEEKK

Poly(ether ether ketone ketone)

PEG

Polyethylene glycol (also PEO)

PEI

Poly(ether imide)

PEK

Poly(ether ketone)

PEKK

Poly(ether ketone ketone)

PEMA

Polyethylmethacrylate

Penton

Poly[3,3-bis(chloromethyl)oxetane]

PET

Polyethyleneterephthalate

PET-b-PS

Block copolymer of PET and PS segments

Phenoxy

Poly(hydroxy ether of bisphenol A)

PI

Di-n-octadecyl ester of itaconic acid

PI

Polyisoprene

PIB

Polyisobutene

PMMA

Polymethylmethacrylate

POM

Polyoxymethylene

PP

Isotactic polypropylene

PPE, PPO

Poly(2,6-dimethyl 1,4-phenylene ether), GE Co. trade name

PPG

Poly(propylene glycol)

PPS

Poly(phenylene sulfide)

PS

Atactic polystyrene

PSMA

Poly(styrene-co-maleic anhydride)

PVAc

Poly(vinyl acetate)

PVC

Polyvinyl chloride

PVDF

Poly(vinylidene fluoride) (sometimes expressed as PVF2)

PVF

Poly(vinyl fluoride)

PVME

Polyvinylmethylether

RIPS

Reaction-induced phase separation

SAN

Poly(styrene-co-acrylonitrile)

SARAN

P(VCl2-VC), P(VCl2-VA), or P(VCl2-AN) random copolymers of vinylidene chloride (VCl2) with vinyl chloride (VC), vinyl acetate (VA), and acrylonitrile (AN), respectively

SBS

Elastomeric styrene-butadiene-styrene triblock polymer (also TR)

SD

Spinodal decomposition

SEBS

Styrene-ethylene/butylene-styrene triblock polymer

SMA

Poly(styrene-co-maleic anhydride)

sPMMA

Syndiotactic poly(methyl methacrylate)

sPS

Syndiotactic polystyrene

TR

Thermoplastic rubber (also SBS)

UHMWPE

Ultra-high-molecular-weight polyethylene

VDF-HFA

Copolymer of vinylidene fluoride and hexafluoro acetone

VDF-TFE

Copolymer of vinylidene fluoride and tetrafluoro ethylene

VLDPE

Very low-density polyethylene

compat.

Compatibilization, compatibilized, etc.

conc.

Concentration

cryst.

Crystallization, crystalline, crystallize

cte

Constant

DSC

Differential scanning calorimetry

etc.

Et cetera

exp.

Exponent

HM

High molecular weight

LCST

Lower critical solution temperature

O. M.

Optical microscopy (also OM)

phr.

Parts per hundred

[(polymer)]

Amount/concentration of the cited polymer

SALS

Small-angle light scattering (also SALLS)

SAXS

Small-angle X-ray scattering

SEM

Scanning electron microscopy

temp.

Temperature

UCST

Upper critical solution temperature

WAXS

Wide-angle X-ray scattering

WLF

Williams, Landel, and Ferry

C 1, C 2, C 3

WLF constants

C-2

Carbon chain with 2 C-atoms; i.e., ethylene

C-3

Carbon chain with 3 C-atoms; i.e., propylene

C p

Heat capacity under constant pressure

E 1

Energy dissipated for rejection of droplets during spherulite growth

E 2

Energy to overcome the inertia of droplets during spherulite growth

E 3

Energy required to form new interfaces when droplets are engulfed

E 4

Energy dissipated for deformation of occluded particles during spherulite growth

F 12

Spreading coefficient

f z (1)

Fraction of dispersed droplets of volume VD that contain z heterogeneities of type 1

G

Isothermal spherulite growth rate

G o

Theoretical spherulite growth rate

G 1

Undisturbed spherulite growth rate of the homopolymer described by the Turnbull-Fisher equation

M (1)

Concentration of heterogeneities of type 1

MW

Molecular weight

n

Avrami exponent

N

Nucleation density

N/S

Nucleation density normalized per unit area

K

Overall crystallization rate

t 0.5

Halftime of crystallization at a fixed T c,iso

T c

Bulk crystallization temperature upon cooling from the melt

T c o

Crystallization temperature of the bulk homopolymer

T c,cold

Cold crystallization temperature

T c,hom

Homogeneous crystallization temperature

T c,i

Crystallization temperature at which heterogeneities of type i become active

T c,iso

Isothermal crystallization temperature

T c,max

Optimal isothermal crystallization temperature which yields the highest overall crystallization

T g

Glass-transition temperature

T m

Measured melting temperature of the crystalline phase

T m o

Theoretical melting temperature for crystalline lamellae of infinite thickness

T m ′

Observed melting temperature of the crystalline phase in blends

T melt

Premelting temperature

t melt

Time the polymer is kept in the melt

V D

Average volume of dispersed polymer droplets

Vol%

Volume percentage

wt%

Weight percentage

X c

Total degree of crystallinity

y p (m, c)

Lateral surface free energy between the crystal and its own melt

y pn (m)

Interfacial energy between the nucleating species and the polymer melt

y pn (c)

Interfacial energy between the nucleating species and the polymer crystal

z

Number of heterogeneities of type 1, inducing crystallization in the bulk polymer at T c o

ΔE

Activation free energy for the transport of chains through the liquid–solid interface

ΔF

Difference of interfacial energies; driving force for rejection, engulfing, and/or deformation of dispersed droplets during spherulite growth

ΔF *

Free energy for the formation of a nucleus of critical size

ΔH m

Total melting enthalpy of the crystalline polymer fraction

ΔT c,hom

Degree of undercooling required for homogeneous crystallization

ΔT c,i

Degree of undercooling required before a heterogeneity of type i can become active

Δy i

Specific interfacial energy difference between a nucleating species of type i and the polymer

Δy pn

Specific interfacial energy difference between a nucleating species and the polymer

γ PS

Interfacial free energy between the crystallizing solid and the inclusions

γ PL

Interfacial free energy between the liquid polymer melt and the inclusions

σ ο

Surface free energy of folding

σ 1,2

Interfacial free energy between two phases of a blend in the melt

σ i,1

Interfacial free energy of an impurity with respect to melt phase 1

σ i,2

Interfacial free energy of an impurity with respect to melt phase 2

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© 2014 Springer Science+Business Media Dordrecht

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Groeninckx, G., Harrats, C., Vanneste, M., Everaert, V. (2014). Crystallization, Micro- and Nano-structure, and Melting Behavior of Polymer Blends. In: Utracki, L., Wilkie, C. (eds) Polymer Blends Handbook. Springer, Dordrecht. https://doi.org/10.1007/978-94-007-6064-6_5

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