JOURNAL OF MATERIALS SCIENCE 22 (1987) 523-531
Drawing of virgin ultrahigh molecular weight
polyethylene: an alternative route to high
strength/high modulus materials
Part 2 Influence of polymerization temperature
PAUL SMITH*, HENRI D. CHANZYt, BRUNO P. ROTZINGER§
E. L du Pont de Nemours and Company, Inc., Central Research and Development Department,
Experimental Station, Wilmington, Delaware 19898, USA
The synthesis of ultra-high molecular weight polyethylene films and the production of high
strength/high modulus tapes and filaments drawn directly from the virgin polymer are described.
The study particularly focuses on the effect of the polymerization temperature on the defor-
mation behaviour of the virgin UHMW polyethylene films. These results are discussed within
the framework of the entanglement concepts for deformation of weakly bonded macromol-
ecules. The develop/nent of the room temperature Young's modulus and the tensile strength
with draw ratio is presented and compared with modulus and tenacity/draw ratio relations
observed for melt and solution crystallized polyethylene.
1. Introduction
The structure and morphology of virgin, i.e. as-
polymerized or nascent, crystallizable polymers has
been a topic of interest in the 1960s [1-5]. In these
early studies it was already recognized that under
certain experimental conditions monomers may sim-
ultaneously polymerize and crystallize into chain-
extended structures. The mechanism underlying this
interesting polymerization is reasonably well under-
stood [1-5]. Macromolecules polymerized below their
melting point, or, rather, dissolution temperature in
the polymerization mixture, never experience the
liberty of the completely liquid state; only a part of the
growing molecule is "dissolved" in its surrounding
medium. The macromolecules thus never adopt a
random coil conformation and, important in relation
to the present work, do not form many entanglements
with neighbouring chains. The actual local tempera-
ture, pressure and concentration determine how many
segments of the growing chain are in the liquid state;
that is true if the polymerization rate does not exceed
the rate at which the polymer segments are incor-
porated into the crystalline solid (schematically illus-
trated in Fig. 1 for Ziegler-Natta type ethylene poly-
merization). Thus it can readily be envisaged that
under selected experimental conditions virgin poly-
mers are produced in which the macromolecules
exhibit a chain-extended and virtually "non-entangled"
conformation. An example of a polymer produced
commercially under such experimental conditions is
poly(tetrafluorethylene) (PTFE) [6-8]. As a result,
virgin PTFE has a number of properties that axe
remarkable in comparison with those of the once-
molten (and re-entangled) polymer: a very high crys-
tallinity, high melting temperature [9] and most
unusual flow characteristics of the solid polymer [10].
In Part 1 [11] we described preliminary results
on drawing of virgin ultra-high molecular weight
(UHMW) polyethylene as an alternative route to high
strength fibres. The presented method dispenses with
the elaborate dissolution, precipitation and solvent
recovery procedures in the "gel-spinning" technique
[12, 13] that axe necessary to untangle the long macro-
molecules prior to tensile drawing [14]. The alternative
virgin-polymer processing technique [11] relies on the
synthesis of polyethylene under experimental con-
ditions where the macromolecules are produced in a
near non-entangled conformation.
In view of the foregoing introductory remarks on
virgin polymers, it is evident that the polymerization
variables, such as temperature and pressure have a
major effect on the conformation of the macromol-
ecules produced and, therefore, on the properties of
the as-polymerized polymer. In this paper we report
on the effect of the polymerization temperature on the
drawing characteristics of virgin UHMW polyethy-
lene.
2. Experimental techniques
Virgin polyethylene films were produced according to
the technique that was previously described [I 1, 15, 16].
A rack containing six cleaned glass slides was immersed
in a boiling solution of 1 mM freshly distilled VCI4 in
dry n-heptane. After 10min a coating of fine VCI3
*Present address: University of California, Materials Program, Santa Barbara, California 93106, USA.
~i Permanent address: CERMAV (CNRS), BP 68, 38402 Saint Martin d'Heres, France.
§Present address: Ciba-Geigy AG, Zentrales Forschungslaboratorium, CH-4002 Basel, Switzerland.
0022-2461/87 $03.00 + .12 © 1987 Chapman and Hall Ltd. 523