You are on page 1of 5

CLINICAL ORTHOPAEDICS AND RELATED RESEARCH

Number 429, pp. 68–72


© 2004 Lippincott Williams & Wilkins

Fatigue Crack Propagation Resistance of Highly


Crosslinked Polyethylene
Letitia Bradford, MD*; David Baker, PhD†; Michael D. Ries, MD‡; Lisa A. Pruitt, PhD§
Downloaded from http://journals.lww.com/clinorthop by BhDMf5ePHKav1zEoum1tQfN4a+kJLhEZgbsIHo4XMi0hCywCX1AWnYQp/IlQrHD3i3D0OdRyi7TvSFl4Cf3VC1y0abggQZXdgGj2MwlZLeI= on 09/27/2021

A higher degree of cross-linking has been shown to improve diostereometric analysis (RSA) techniques show less pen-
wear properties of ultra-high molecular weight polyethylene etration of the femoral head into the acetabular liner of
in laboratory studies. However, cross-linking can also affect highly cross-linked UHMWPE compared with conven-
the mechanical properties of ultra-high molecular weight tional UHMWPE.8
polyethylene. Fatigue crack propagation resistance was de-
Although cross-linking improves the wear resistance of
termined for electron beam cross-linked ultra-high molecu-
lar weight polyethylene and compared with gamma irradia-
UHMWPE, its mechanical properties also are affected.
tion cross-linked and noncross-linked polyethylene fatigue The higher degree of cross-linking causes a restriction of
specimens. Crosslinking was done with different dosages of chain mobility in the amorphous region of the polymer and
irradiation followed by melting. For one irradiation dose (50 results in limited plasticity in the polyethylene (PE). This
kGy) extrusion and molding processes were compared. A decreased tendency toward plastic damage is thought to be
fracture mechanics approach was used to determine how the the primary mechanism for improving the wear resistance
degree of cross-linking affects resistance to crack propaga- of UHMWPE. It is thought that cross-linking mitigates
tion in ultra-high molecular weight polyethylene. Fatigue texture evolution and cyclic softening in the polymer.5,15
crack propagation resistance was reduced in proportion to However, this lack of plasticity could be detrimental to
the irradiation dose. The type of irradiation (gamma or elec- other mechanical properties such as toughness, ductility
tron beam) or manufacturing method (extrusion or molding)
and fatigue resistance.
did not affect fatigue crack propagation resistance. The re-
duced fatigue strength of highly cross-linked ultra-high mo-
Compared with unsterilized UHMWPE, the mechanical
lecular weight polyethylene could lead to mechanical failure properties including yield strength, ultimate tensile
in conditions that are associated with cyclic local tensile strength, and elongation are reduced by cross-linking. Re-
stresses. sistance to fatigue crack propagation also is decreased by
cross-linking.1–3
The loads on a modular UHMWPE acetabular liner
are primarily compressive so a reduction in mechanical
Highly cross-linked ultra-high molecular weight polyeth-
properties of UHMWPE may not result in mechanical fail-
ylenes (UHMWPEs) have been developed in an effort to
ure. However, tensile stresses may also occur particularly
minimize wear in total hip arthroplasty (THA). Cross-
at the liner-locking mechanism and during activities that
linking improves the abrasion resistance of UHMWPE.
are associated with impingement of the femoral neck
Hip simulator studies consistently show decreased wear of
against the UHMWPE rim. Liner-locking mechanism dis-
highly cross-linked UHMWPE compared with conven-
sociation has been reported as a complication of many
tional UHMWPE.4,5,9,10,12 Early clinical reports with ra-
modular acetabular components.6,11,14 Therefore, the me-
chanical properties of an acetabular liner should be suf-
ficient to minimize the risk of liner-locking mechanism
From the *University of California, San Francisco, CA; †Exxon-Mobil
Corp., Houston, TX; ‡Department of Orthopaedic Surgery, University of failure.
California, San Francisco, CA; §Department of Mechanical Engineering, Gamma irradiation induced cross-linking is associated
University of California, Berkeley, CA. with a reduction in the fatigue crack propagation resistance
The institution of the authors have received funding in support of this study
from Sulzer, Inc. and Depuy, Inc. that is related to the irradiation dose.1,3 The purpose of this
Correspondence to: Michael D. Ries, M.D., Department of Orthopaedic study was to determine the effect of electron beam and
Surgery, University of California, San Francisco, 500 Parnassus Ave. gamma irradiation induced cross-linking on the resistance
(MU 320-W), San Francisco, CA 94143. Phone: 415-502-2235; Fax: 415-
476-1304; E-mail: riesm@orthosurg.ucsf.edu. to propagation of flaws or defects under controlled cyclic
DOI: 10.1097/01.blo.0000150124.34906.34 stresses.

68
Number 429
December 2004 Highly Crosslinked Polyethylene Fatigue 69

MATERIALS AND METHODS

The fatigue crack propagation resistance of Durasul and Sulene


(Sulzer Orthopaedics, Incorporated, Austin, TX) were evaluated
and compared with gamma-irradiation cross-linked UHMWPE
with irradiation doses from 50 kGy (5Mrad) to 200 kGy
(20Mrad). Sulzer Orthopaedics Incorporated supplied the fatigue
fracture specimens of the Sulene and Durasul materials. Sulene
and Durasul have the same base resin (GUR 1020) and are
machined from the same material (compression-molded sheet);
however Sulene is manufactured and distributed as a noncross-
linked polymer, whereas Durasul has radiation cross-linking.
The Durasul proprietary cross-linking procedure uses approxi-
mately 100 kGy of electron-beam radiation at a temperature
below the melt, followed by a melt annealing process at approxi-
mately 150°Celsius.16 The Durasul and Sulene go through eth-
ylene oxide sterilization in a similar fashion. For comparative
purposes, the data were evaluated with a varied range of cross-
linked doses (50 kGy, 100 kGy, and 200 kGy) achieved through
gamma radiation.3 For two doses, 50 kGy and 100 kGy, the
effects of gamma radiation and electron-beam radiation were
compared. Further, for the 50 kGy gamma radiation dose, two Fig 1. Schematic illustration of the compact tension specimen
manufacturing processes were studied: extrusion and molding. used in the fatigue studies is shown.
For the 50 kGy and 100 kGy doses, gamma and electron-beam
cross-linking conditions were examined. In extruded, nonsteril-
ized form, GUR 1050 served as the control for this study. In
these comparison studies cross-linking was done using gamma The compact tension specimens were subjected to tension
or electron beam radiation in an inert environment, then brought fatigue loading to examine the crack growth inception and
above the melt temperature and cooled slowly to annihilate free propagation characteristics. Changes in flaw size, a, were mea-
radicals. The test conditions for these material groups were iden- sured as a function of fatigue cycles, N, to determine crack
tical to those for Sulene and Durasul specimens. For all sample growth rate, da/dN. Corresponding stress intensity ranges,
groups, compact tension specimens were machined from cross- ⌬K, were determined (from linear elastic fracture mechanics
linked or control (noncross-linked) rod stock material. Ten assumptions) using ⌬K ⳱ ⌬␴(a)1/2 •f(a/W), where ⌬␴ is the
samples were evaluated for each group. cyclic stress range, a is the flaw size, and f(a/W) is the geometric
All fatigue tests were done on compact tension specimens factor for the compact tension specimen. The stress inten-
with the following geometry: width, W ⳱ 25.4 mm; length, L ⳱ sity range necessary for a minimum growth rate of 10−6 mm per
31.75 mm; height, 2H ⳱ 31.75 mm; initial notch length, a ⳱ cycle was identified as ⌬⌲incep3, and determined for each
8.89 mm; notch angle, ␪ ⳱ 60°; hole diameter, d ⳱ 5.334 mm; specimen group. This value has been chosen to compare critical
and thickness, B ⳱ 8.13 mm. An illustration of the specimen values for stable crack propagation and serves as a parameter to
geometry is provided in Figure 1. The tests were done in a measure differences between fatigue crack propagation resis-
recirculating deionized water bath maintained at body tempera- tance in UHMWPE materials.2 In addition, the crack propaga-
ture (37°C). Samples were allowed to equilibrate for one hour in tion rates were characterized as a function of stress intensity
the bath before testing. An Instron 8511 (Instron Corp., Canton, range, da/dN versus ⌬K. Fatigue tests were concluded when
MA) servohydraulic materials testing machine was used to con- the crack became too large to control test parameters (this typi-
duct the fatigue tests. Cyclic loading was applied using a sinu- cally occurred at a crack velocity near 10−2 mm per cycle, which
soidal waveform at a frequency of 5 Hz. This frequency has been is outside of the linear crack growth region.) At the comple-
confirmed to produce negligible hysteretic heating in previous tion of each fatigue characterization study, fractography was
studies.3 Tension fatigue tests were done using pin loading at a done using the JEOL JSM 6300 scanning electron microscope
load ratio (the ratio of the minimum load to the maximum load) to examine the fracture micromechanisms for each material
of R ⳱ 0.1. All specimens were razor notched before the tension group.
fatigue tests to establish a sharp mode I crack. All fatigue Each of the specimens tested has a variable crack length. The
samples had initial conditions of a/W approximately equal to 0.3. ⌬⌲incep of each specimen tested is dependent on the crack length
The initial stress intensity was kept constant in tests before crack and material properties so that a number of specimens are needed
inception to control for variations in initial crack length. The to determine the ⌬⌲incep value for each material. Because there
length of the fatigue flaw was measured using an Olympus BH-2 is one ⌬⌲incep value obtained for each material group, statistical
(Olympus Optical Co., Melville, NY) optical microscope with comparisons of ⌬⌲incep values between groups were not pos-
resolution of 0.2 ␮m. sible.
Clinical Orthopaedics
70 Bradford et al and Related Research

RESULTS

Fatigue crack propagation resistance was decreased by


cross-linking. The fracture fatigue analysis of Sulene and
Durasul resulted in ⌬Kincep of 1.7 and 0.65 MPa√m, re-
spectively. Table 1 summarizes the ⌬Kincep values and
slope m of Durasul and Sulene.
Evidence of ductile behavior of the polymer resulting in
blunting of the crack tip was seen as a crisscross pattern in
scanning electron micrographs of the fracture specimens.
Figure 2 shows representative scanning electron micro-
graphs of cross-linked specimens exposed to varied de-
grees of radiation.2 Note the reduction of ductile, criss-
cross tearing on the fracture surfaces as the dose of irra-
diation and degree of cross-linking increase.
Fatigue crack propagation resistance decreased in pro-
portion to the irradiation dose or amount of cross-linking.
Figure 3 shows a plot of crack propagation rate, da/dN, as
a function of stress intensity range, ⌬K, for Durasul and
Sulene. For comparison, the fatigue crack propagation data
for GUR 1050 at crosslink dosages of 50, 100, and 200
kGy through gamma radiation along with a control (non-
cross-linked GUR 1050)2 are provided in this plot.
The fatigue crack propagation resistance was not af-
fected by the manufacturing method (molding or extru-
sion) or type of irradiation used (gamma or electron
beam). Figure 4 provides a plot of the 50 and 100 kGy
through gamma radiation and electron beam radiation, the
50 kGy gamma irradiated molded and extruded samples,
and the noncross-linked control.
The fatigue crack propagation resistance decreases with
increasing crosslink dose independent of irradiation source
or manufacturing method (Table 1). The Durasul ⌬Kincep
value and slope are very similar to the 100 kGy data. Also
note that the Sulene fatigue behavior is similar to that of
the control noncross-linked PE control.

TABLE 1. Summary of Fatigue Crack Propagation


Inception Values, ⌬Kincept (MPa √m) for
All Materials
⌬Kincept
Materials Groups (MPa √m)
Control (GUR 1050, noncross-linked, extruded) 1.76
Sulene (GUR 1020, noncross-linked) 1.7
Durasul (GUR 1020, 100kGy, E-beam) 0.65
50kGy (GUR 1050, gamma, extruded) 0.91
50kGy (GUR 1050, E-beam, extruded) 0.81
50kGy (GUR 1050, gamma, molded) 0.92
100kGy (GUR 1050, gamma, extruded) 0.72
100kGy (GUR 1050, E-beam, extruded) 0.71 Fig 2. Representative micrograph of the Paris regime for (A)
noncross-linked control, (B) 50 kGy gamma radiation, and (C)
E-beam = electron beam 100 kGy gamma radiation are shown.
Number 429
December 2004 Highly Crosslinked Polyethylene Fatigue 71

Fig 3. Fatigue crack propagation


rate as a function of stress intensity
range is shown.

DISCUSSION the PE is caused by a loss of plasticity. Studies have shown


that this reduction in ductility is accompanied by less la-
The degree of cross-linking in UHMWPE is achieved by mellae tearing in the polymer.13 This raises the question of
controlling the dose of irradiation that the polymer is ex- whether this can be extrapolated to initiation of fatigue
posed to under specific processing conditions. Each ortho- cracks in vivo. In order for cross-linking to be beneficial to
paedic manufacturer follows a unique proprietary protocol the longevity of the device, it is presumed that the devices
to achieve cross-linked PE. In general, highly crosslinked are without flaws before and during their implantation.
UHMWPE is attained using a minimum of 50 to100 kGy Ductile tearing of the polymer causes blunting of the
(5–10 Mrad) of gamma9 or electron-beam12 radiation. This crack tip, slowing progression of a fatigue crack. Fractog-
is typically done below the melt temperature of the poly- raphy of the cross-linked fatigue specimens show a de-
mer and then is coupled with a secondary annealing treat- creased prevalence of crisscross patterns, indicating a lack
ment to neutralize any remaining free radicals produced by of ductile tearing, with increased irradiation dose. Frac-
irradiation. Cross-linking is known to change the molecu- tography of noncross-linked UHMWPE after having fa-
lar structure of the PE; for example, some cross-linked tigue crack propagation, shows classic crisscross patterns
UHMWPE materials have a decreased crystallinity (∼20– that are associated with ductile tearing.3 Baker et al2 have
30%) compared with the standard 1050 materials shown that the fracture surface of cross-linked PE often
(∼50%).12 Cross-linking can also be achieved through per- has a more brittle appearance and shows a decreased pro-
oxy-based chemistry using a minimum of 0.3–0.5% per- pensity for ductile tearing. Although ductile tearing has
oxide,7 but the question of its long-term stability has lim- been seen in nascent PE and at reduced levels of irradia-
ited its application as an orthopaedic biomaterial. tion used for sterilization, it is often diminished further
Laboratory testing indicates that cross-linked with higher irradiation doses (such as used for cross-
UHMWPE has reduced resistance to fatigue crack propa- linking PE.)
gation.1 Baker et al2 have shown that chemical and radia- The reduced fatigue crack propagation resistance of
tion cross-linking results in a lower value of stress inten- highly cross-linked PE could lead to mechanical failure in
sity necessary for the growth of a flaw compared with vivo under conditions associated with cyclic tensile stress.
noncross-linked UHMWPE. However, it has also been Although stresses in a modular UHMWPE actetabular in-
suggested that cross-linking is beneficial to the flaw ini- sert primarily are compressive, tensile stresses may occur
tiation resistance.2 The diminished capacity for flaws in at the liner-locking mechanism and along the rim of the
Clinical Orthopaedics
72 Bradford et al and Related Research

Fig 4. Fatigue crack propagation


rates of gamma-irradiated and elec-
tron-beam irradiated and extruded
and molded specimens are shown.

component if impingement occurs. Range of motion to 7. Kurtz SM, Muratoglu OK, Evans M, et al: Advances in the pro-
cessing, sterilization, and crosslinking of ultra-high molecular
impingement carefully should be evaluated with any liner weight polyethylene for total joint arthroplasty. Biomaterials
material used in total hip arthroplasty including highly 20:1659–1688, 1999.
cross-linked PE and liner locking mechanisms should be 8. Martell JM, Verner JJ, Incavo SJ: Clinical performance of a highly
cross-linked polyethylene at two years in total hip arthroplasty: a
designed to minimize the risk of mechanical failure under randomized prospective trial. J Arthroplasty 18:55–59, 2003.
cyclic loads. 9. McKellop H, Shen FW, Lu B, et al: Development of an extremely
wear-resistant ultra high molecular weight polyethylene for total hip
replacements. J Orthop Res 17:157–167, 1999.
References 10. McKellop H, Shen FW, Lu B, et al: Effect of sterilization method
1. Baker D, Hastings R, Pruitt L: A Study of the Fatigue Resistance of and other modifications on the wear resistance of acetabular cups
Chemical and Radiation Crosslinked Medical Grade UHMWPE. made of ultra-high molecular weight polyethylene. A hip-simulator
J Biomed Mater Res 46:573–581, 1999. study. J Bone Joint Surg 82A:1708–1725, 2000.
2. Baker DA, Bellare A, Pruitt L: The effects of degree of crosslinking 11. Mihalko WM, Papademetriou T: Polyethylene liner dissociation with
on the fatigue crack initiation and propagation resistance of ortho- the Harris-Galante II acetabular component. Clin Orthop:166, 2001
pedic-grade polyethylene. J Biomed Mater Res 66A:146–154, 2003. 12. Muratoglu OK, Bragdon CR, O’Connor DO, et al: A novel method
3. Baker DA, Hastings RS, Pruitt L: Compression and tension fatigue of cross-linking ultra-high-molecular-weight polyethylene to improve
resistance of medical grade ultra high molecular weight polyethyl- wear, reduce oxidation, and retain mechanical properties. Recipient of
ene: the effect of morphology, sterilization, aging and temperature. the 1999 HAP Paul Award. J Arthroplasty 16:149–160, 2001.
Polym 41:795–808, 2000. 13. Shen FW, McKellop HA, Salovey R: Irradiation of chemically
4. Edidin AA, Kurtz SM: Influence of mechanical behavior on the crosslinked ultrahigh molecular weight polyethylene. J Polym Sci
wear of 4 clinically relevant polymeric biomaterials in a hip simu- Part Polym Phys 34:1063–1077, 1996.
lator. J Arthroplasty 15:321–331, 2000. 14. Udomkiat P, Dorr LD, Wan Z: Cementless hemispheric porous-
5. Edidin AA, Pruitt L, Jewett CW, et al: Plasticity-induced damage coated sockets implanted with press-fit technique without screws:
layer is a precursor to wear in radiation-cross-linked UHMWPE average ten-year follow-up. J Bone Joint Surg 84-A:1195–2000, 2002.
acetabular components for total hip replacement. Ultra-high- 15. Wang A: Wear of ultra-high molecular weight polyethylene acetab-
molecular-weight polyethylene. J Arthroplasty 14:616–627, 1999. ular cups in a physiological hip joint simulator in the anatomical
6. Gonzalez Della Valle A, Ruzo PS, Li S, et al: Dislodgment of position using bovine serum as a lubricant. Proc Inst Mech Eng [H]
polyethylene liners in first and second-generation Harris-Galante 212:71–72, 1998.
acetabular components. A report of eighteen cases. J Bone Joint 16. www.sulzerorthopedics.com: The Durasul Tribological system, ac-
Surg 83-A:553–559, 2001. cessed on 11/30/01.

You might also like