Journal of Dental Research

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A Non-destructive Method of Evaluating the Elastic Properties of Anterior

Restorative Materials
R. Whiting and P.H. Jacobsen
J DENT RES 1980 59: 1978
DOI: 10.1177/00220345800590110901

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A Non-destructive Method of Evaluating the Elastic
Properties of Anterior Restorative Materials
R. WHITING and P. H. JACOBSEN*
Department of Biomedical Engineering, King's College Hospital Medical School, Dulwich Hospital,
London, SE22 8PT
An ultrasonic pulse transit-time method was used
to deternine the Young's modulus, shear modulus,
and Poisson's ratio of seven anterior-restorative
materials. Small rectangular specimens were im-
mersed in a water bath and ultrasonic pulses prop-
agated through them. Two types of ultrasonic wave
could be generated inside the specimen by altering
the angle of incidence. Measurement of the pulse
transit-time for these two waves enabled their
velocities and, hence, the material's elastic con-
stants to be calculated. The variation of these
properties with time of conditioning and tempera-
ture was also determined.
J Dent Res 59(1 1):1978-1984, November 1980
Introduction.
The laboratory assessment of the mechanical
properties of composite restorative materials
presents considerable difficulty. This is
due mainly to the high stiffness of the ma-
terials, the visco-elastic nature of the resin
base, and the need to use clinically realistic
specimen sizes.
It has been common practice to test the
dental composites using destructive (or
"static") test methods. 1-3 While valuable for
determining ultimate strengths, these meth-
ods are not well suited to measuring elastic
properties. Small changes in length are diffi-
cult to record; a clear indication of the time-
dependent nature of the elasticity is not
given, and the size and shape of the speci-
mens can influence the results.4
It is now common in materials science to
use non-destructive (or dynamic) methods
to assess polymeric materials.5 These meth-
ods impose a very small cyclic stress on the
material at a well-defined rate.
Received for publication October 26, 1979
Accepted for publication February 25, 1980
Reprint requests: Department of Conservative
Dentistry, Welsh National School of Medicine,
Heath Park, Cardiff, Wales
Based on a paper presented at the IADR,
British Division meeting, April, 1979
1978
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One such method, described by the pres-
ent authors,6 is the determination of the
response of a material to low frequency
torsional oscillations using a torsion pendu-
lum.
This present paper describes another non-
destructive technique, the ultrasonic pulse
transit-time method, which tests the re-
sponse of a material to high frequency
oscillation.7 Ultrasound is used to stress the
material, and the modulus of elasticity is
derived from measurements of the velocity
of the ultrasound inside the specimen.
This method has been used to evaluate
many different types of polymer.8'9 It has
also been used for fiber-reinforced poly-
mers.10 However, little work has been re-
ported on its use for particulate composites.
In the present study, six dental composites
and one unfilled dental resin were tested
using pulsed ultrasound. The Young's and
shear moduli and Poisson's ratio were
determined. The variation of these proper-
ties with time of conditioning and tempera-
ture was also recorded.
Materials and methods.
Two major types of wave can exist in an
isotropic solid. These are longitudinal and
transverse waves. If a specimen is positioned
with its surface perpendicular to the direc-
tion of the incident waves, longitudinal
waves are generated inside the material.
If, however, the specimen is rotated so that
the angle of incidence of the waves is greater
than a certain so-called "critical" angle, then
transverse waves are generated in the mater-
ial. To determine the elastic moduli of the
material, it is necessary to measure the
velocities of the two types of wave.
In the ultrasonic pulse transit-time
method, the two velocities are calculated
from measurements of the time taken for
pulses to travel through the specimen.
However, several problems are introduced by
the small specimen size. First, the theory
Vol. 59 No. 11 NON-DESTRUCTIVE EVALUA TION OFRESTORA TIVE MATERIALS
associated with this method assumes plane
wave conditions. For plane waves to exist
inside the specimen, it is necessary that the
wavelength of the ultrasound should be
small compared with the dimensions of the
specimen. Second, the ultrasonic beam must
be very narrow, and third, the time taken for
a pulse to traverse a specimen approximately
1 mm in thickness is of the order of 10-7
seconds. Therefore, a very accurate timing
system is required.
A frequency of 5MHz was chosen for this
study. Lower frequencies would not satisfy
the plane wave conditions, and it was con-
sidered that higher frequencies would
lead to unacceptably high absorption of the
ultrasound.
Small ultrasonic probes were constructed
using square plates (2 mm x 2 mm) of lead
zirconate titanate piezoelectric ceramic. *
The probe design is shown in Fig. 1. The
front surface of the ceramic was coated with
a thin film of epoxy resin. It was considered
that the effect of this film on the perform-
ance of the ceramic would be extremely
small. The resin layer was extended over the
end of the acrylic tube to provide a water-
tight seal. The rear surface of the ceramic
was in contact with a backing material which
consisted of tungsten-filled epoxy resin.
This material is a good absorber of ultra-
soundll and also rapidly damps the vibra-
tion of the ceramic. The shape of the ultra-
sonic beam produced by these probes was
analyzed, and a typical profile is shown in
Fig. 2.
Acrylic case
Piezoelectric
ceramic
Fig. 1 -Ultrasonic probe design.
*Unilator Type PC5, Unilator Technical Cera-
mics, Wrexham, Clwyd, Wales
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1979
The complete ultrasonic system is shown
diagrammatically in Fig. 3. The pulse genera-
tor provided electrical pulses which were
used to excite the transmitting probe. This
probe converted the electrical signals into
ultrasonic pulses. These were then propa-
gated through a specimen and detected by
a receiving probe. The probes and specimen
were immersed in a water bath at a tempera-
ture of 230 ± 0.20C.
The receiving probe reconverted the ultra-
sonic pulses to electrical pulses, and these
were amplified and displayed on an oscillo-
scope. The oscilloscope' had a built-in 100
MHz counter and LED display. This pro-
vided a direct digital readout of the time
taken for pulses to travel around the circuit
(the total transit-time). This measurement
could be made to an accuracy of + 2 nano-
seconds.
1cm
3dB steps of
Near field Far field transmitted power
Fig. 2 -Ultrasonic beam profile
Amplifier
Oscilloscope / Timer
Fig. 3 -The complete system.
The specimen was then removed, and,
with the pulses passing through water only,
a second total transit-time was measured.
The difference in these transit-times was
due to the difference between the time
taken for pulses to traverse the specimen and
+Hewlett Packard Model No. 1743A, Hewlett
Packard Co., CO
1980 WHITING & JACOBSEN J Den t R es Novem ber 1 980

the time taken to traverse an equivalent 1. Beam specimens 1 mm in thickness, 3 mm

distance in water. Therefore, by measuring
the thickness of the specimen and using
standard values12 for the velocity of ultra-
sound in water at the experimental tempera-
ture, it was possible to calculate the velocity
of ultrasound in the test-material. This pro-
cedure was repeated for the two types of
wave.
The effects of inhomogeneities on the
propagation of ultrasound through a mater-
ial are averaged providing that the inhomo-
geneities are small compared to the wave-
length of the ultrasound and that they are
evenly distributed.9 For 5 MHz ultrasonic
waves propagating through composite speci-
mens which had been prepared by thorough
mixing, it was reasonable to assume that the
above conditions were satisfied. Therefore,
it was possible to consider all the materials
to be homogeneous and isotropic. To cal-
culate the Young's and shear moduli and
Poisson's ratio, the standard formula12
for such materials were used:
in width, and 20 mm in length were pre-
pared. Specimen dimensions were measured
with a micrometer gauge to an accuracy of
± 0.5%. Six specimens of each material
were conditioned at 600C for 24 h to
ensure a complete cure. For each of mater-
ials, Co and I, four further specimens were
prepared and conditioned in this way and
were then placed in water at 370C. These
were tested after one, three, seven, and 28
d of conditioning to evaluate the effects of
water absorption.
Four further specimens of materials Co
and I were prepared and conditioned at
600C for 24 h. The Young's modulus was
then determined as a function of tempera-
ture from 200C to 750C. These materials
were selected because their formulations
were considered to be representative of the
two different types of composite, the
conventional type and the microfine type.
Some comparative data were available also.

Young's modulus Y = pv2 -k2

Results.
For all the materials tested, a strong
Shear modulus G = pvT2 clear signal was present at the receiving
Poisson's ratio k2- 2 probe. An effective absorption, measured by
2 (k2 -1) comparing the amplitudes of transmitted
and received pulses, was typically 3
K = VL dBmm-1.
where
VT The Young's modulus determined for
VL = longitudinal velocity three standard materials, aluminum, brass,
VT = transverse velocity and polymethylmethacrylate (PMMA), is
p = specimen density.
shown in Table 2. The variation of modulus
with thickness for PMMA was not significant
The materials studied are shown in Table (Student's t test p > 0.05).
TABLE 1
MATERIALS STUDIED
Material Code Type Batch Number Manufacturer
Adaptic A Bis GMA Composite 6F018 Johnson & Johnson, NJ
Concise C Bis GMA Composite 7251J13/7251L8 3M Company, MN
Cosmic Co Bis GMA-Urethane SAllSB/ Amalgamated Dental Co.,
Acrylate Composite SA8SB London
Isopast I Bis GMA Composite 290377 Vivadent, Leichtenstein
with Low Filler
Content
Orthofil 0 Unfilled PMMA 004JI/OO1El Dental Fillings, Ltd., London
Prestige P Aromatic Dimeth- HPRO109/ Lee Pharmaceuticals, CA
acrylate Composite HPRO110
T. D. 71 T PMMA Composite 29EJ/00201 Dental Fillings, Ltd., London

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Vol. 59 No. 11 NON-DESTRUCTIVE EVALUATION OFRESTORA TIVE MATERIALS 1 981

The moduli and Poisson's ratio deter- Discussion.

mined ultrasonically for the dental materials
are shown in Table 3. Table 4 shows the
effect of conditioning in water at 37cC. The
temperature of testing for these two tests
was 230C.
Fig. 4 shows the variation of the modulus
of material Co with temperature. Similar
curves were obtained for material I.
An absorption of 3 dBmm- 1 for the
composites compares well with that reported
by Greener et al., 17 although these authors
gave no information on the method of
measurement. This absorption is surprisingly
low. The presence of many phase boundaries
within a composite material and the large

TABLE 2
YOUNG'S MODULUS DETERMINED FOR THREE STANDARD MATERIALS AND
COMPARED WITH LITERATURE VALUES
Specimen Young's modulus
Thickness (mm) Ultrasound Ultrasound Static Tests
Material (this study) (this study) (literature values) (literature values)
Aluminum 3.05 68.7 + 1.2 71.012 69 - 7114
1.25 68.3 + 0.9 68 - 7115
Brass 3.05 101.1 + 1.9 10012 103.514
0.72 100.2+ 1.9 97 - 11015
PMMA 3.01 6.3 ± 1.9 5.312 2.4- 3.514
1.51 6.2 + 0.1 5.78 2.4 - 3.816
0.44 6.1 + 0.2 6.213

TABLE 3
YOUNG'S MODULUS, SHEAR MODULUS, AND POISSON'S RATIO FOR SPECIMENS
CONDITIONED AT 600C FOR 24 H, AND TESTED AT 230C
Material E(GNm-2) + S.D. G(GNm-2) + S.D. v
A 24.50 + 0.41 9.96 + 0.12 0.23
C 24.55 + 0.42 9.82 ± 0.40 0.25
Co 23.90 + 0.30 9.41 + 0.21 0.27
I 7.41 ± 0.05 2.81 + 0.02 0.32
0 5.60 + 0.26 2.12 + 0.09 0.32
P 27.10 + 0.40 10.80 + 0.30 0.26
T 12.02 + 0.09 4.66 ± 0.03 0.29

TABLE 4
VARIATION OF THE ULTRASONIC VELOCITIES, MODULI, AND POISSON'S RATIO
WITH TIME OF CONDITIONING. SPECIMENS CONDITIONED IN WATER AT
370C. TESTS PERFORMED AT 230C.
Material Time VL(msec-l) VT(msec-1) E(GNm-2) G(GNm-2) v
One d 3642 2008 23.81 9.27 0.28
Three d 3601 1984 23.26 9.05 0.28
Co One wk 3582 1976 23.03 8.98 0.28
Four wk 3573 1970 22.91 8.93 0.28
One d 2854 1435 7.10 2.67 0.33
Three d 2810 1433 7.04 2.66 0.32
I One wk 2770 1411 6.83 2.58 0.32
Fourwk 2701 1398 6.67 2.53 0.32

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1982 J Dent Res November
WHITING & JACOBSEDR m 1 980
28
y an ultrasonic value of 17 GNm-2. Greener
24
20
Modulus
16
GN m
12
G
8
4 It would appear, therefore, that the
10 20 30 40 50 60
Temperature
Fig. 4- Variation of Young's and shear moduli
of material Co with temperature.
difference in acoustic impedence between
the two phases might be expected to result
in a considerably higher absorption than
this. Two factors may contribute to the low
absorption. First, filler-particle agglomera-
tion would result in fewer phase boundaries.
Second, scattering from discontinuities is
high only when the size of those discontinui-
ties is equal to or larger than the wavelength
of the ultrasound. Therefore, voids, filler
particles, and particle agglomerations less
than 100 Mm in diameter may not contribute
significantly to the scattering loss.
The moduli of the three standard mater-
ials were in good agreement with the litera-
ture values. The modulus of a viscoelastic
material such as PMMA is higher when
measured at ultrasonic frequencies than the
value found using low frequencies or static
tests. This is because the modulus of this
type of material is both strain-rate- and
strain-amplitude-dependent. The greater the
rate of loading and the lower the total load,
the higher the material's stiffness. In ultra-
sonic tests, the rate of strain is high and the
strain amplitude is low. (This amplitude is
approximately 10-5, compared with 10-2
induced by static tests.)
The moduli of the composites are also
high compared to static values. For example,
values of 10.27 and 16.9 GNm-2 have
been reported1,18 for the Young's modulus
of material A measured in static compres-
sion, and 10.8 GNm-2 for this modulus
measured in flexure.19 Barton et al.20 have
compared static and ultrasonic tests of the
Young's modulus of "an experimental
radiopaque material" (a composite based on
a modified dimethacrylate resin). They
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obtained a static value of 9.6 GNm-2 and
et al., 17 in their ultrasonic evaluation of
the composites, measured only one ultra-
sonic velocity, and therefore no modulus
values were obtained. The longitudinal
velocity in materials Co and T was 3265
and 3080 msec- 1, respectively, compared
with 3601 and 3320 msec-1 for this study.
values obtained are a realistic evaluation of
70 80 90 the low strain-, high strain-rate, elastic prop-
0
C
erties of these materials.
The ranking of the moduli reflects the
composition of the materials. Those based
on aromatic dimethacrylate resins and with
a high filler content (A, C, Co, and P) have
the highest moduli. The unfilled resin (0)
and the dimethacrylate resin with a low filler
content (I) have the lowest moduli. It is
interesting to note that, although material I
contains 23% inorganic filler, by weight its
modulus is only slightly higher than the
unfilled methacrylate resin (0).
The value of Poisson's ratio for the un-
filled resin is in approximate agreement with
published values.12'21 Generally, the values
for the composites are lower than the resin
value, probably because of the - low Pois-
son's ratio of glass.21
Conditioning in water reduced the moduli.
There are several mechanisms for water
absorption by composite materials, including
diffusion-controlled absorption by the
resin,21 capillary action (due to voids at the
matrix-filler interface), and general poros-
ity.22 The water absorbed by materials Co
and I has a small plasticizing effect (Table
4). The slightly greater percentage reduction
in modulus for material I is probably due to
the greater proportion of organic resin in
this composite.
The temperature trial indicated no transi-
tion, but a fairly rapid drop in modulus
with temperature did occur. This drop might
suggest a low transition temperature, al-
though a previous study at higher tempera-
tures showed no transition for the composites
and indicated a highly crosslinked structure.6
In this study the more rapid decrease in
modulus may have been due to uptake of
water during the test, even though the time
of testing was short compared with the
water-absorption test (Table 4). Braden24
has shown that the diffusion coefficient of
acrylic resins increases very rapidly with
Vol. 59 No. 11 NON-DESTRUCTIVE EVALUATION OF RESTORA TIVE MATERIALS
temperature, and therefore it is probable
that the materials studied here also have an
enhanced water absorption at elevated tem-
peratures. This condition is similar to that
which would occur clinically.
This work has shown that the ultrasonic
pulse transit-time method is well suited to
the analysis of the resin-based dental restora-
tive materials. Their elastic properties have
not previously been determined in this way.
The modulus values obtained are high com-
pared to static values. This reflects the low
strain-, high strain-rate nature of the test.
The method is potentially very accurate;
the tests are simple to perform, and the
measurements may be made rapidly. The
variation of elastic properties with water
conditioning and with temperature is also
readily determined. The non-destructive
nature of the test leads to considerable econ-
omy both in time and in use of materials.
Furthermore, the results may be related to
those from other types of dynamic tests to
give a greater understanding of the molec-
ular mechanisms responsible for the observed
mechanical response.6'25
In its present form, the method is not
suited to the in vivo measurement of mater-
ial changes during use since considerable
modification would be required to achieve
reliable coupling between the probes and the
tooth, particularly if transverse ultrasonic
waves were to be generated. However, since
the acoustic properties of enamel and dentin
are well documented,26 this method could
readily be extended to the in vitro assess-
ment of restorations and of the effects of
various immersion media on those restora-
tions.
REFERENCES
1. HANNAH, C.M.D. and COMBE, E.C.: Me-
chanical Properties of Composite Restorative
Materials, Brit Dent J 140:167, 1976.
2. BOWEN, R.L. and RODRIGUEZ, M.S.:
Tensile Strength and Modulus of Elasticity of
Tooth Structure and Several Restorative
Resins,JADA 64:85-86, 1962.
3. MACCHI, R.L. and CRAIG, R.G.: Physical
and Mechanical Properties of Composite
Restorative Materials, JADA 78:328-334,
1969.
4. DAVIS, D.M. and JACOBSEN, P.H.: Mechan-
ical Properties of Anterior Restorative Mater-
ials, JDent Res 56:D107, 1977.
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5. FERRY, J.D.: Viscoelastic Properties of
Polymers, 2nd ed., New York: John Wiley,
1970.
6. WHITING, R. and JACOBSEN, P.H.: Dynam-
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7. MARKHAM, M.F.: Measurement of Elastic
Constants by the Ultrasonic Pulse Method,
Brit J Appl Physics, Suppl. 6, S56-S6 3, 195 7.
8. HARTMANN, B. and JARZYNSKI, J.:
Immersion Apparatus for Ultrasonic Meas-
urement in Polymers, J Acoust Soc Amer
56(5):1469-1477, 1974.
9. THOMAS, K. and MEYER, D.E.: Ultrasonic
Measurement of Reproductability and Aniso-
tropy of Processed Polymers, Plastics and
Rubber 1(3/4):136-144. 1976.
10. MARKHAM, M.F.: Measurement of the
Elastic Constants of Fiber Composites by
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11. REID, A.: A Review of Ultrasonic Probe
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12. FILIPCZYNSKI, L.: Ultrasonic Methods of
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1966.
13. ASAY, J.R.; LAMBERSON, D.L.; and
GUENTHER, A.H.: Pressure and Tempera-
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Polymethyl Methacrylate, J Appl Physics
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14. WEAST, R.C.: CRC Handbook of Chemistry
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15. MARKS, L.S.: Mechanical Engineers' Hand-
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Ltd., 1941.
16. PEYTON, F.A.: Restorative Dental Materials,
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17. GREENER, E.H.; WATTS, D.C.; and COMBE,
E.C.: Ultrasonic Evaluation of Anterior
Restorative Materials, J Dent Res 58:543,
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18. DENNISON, J.B. and CRAIG, R.G.: Phys-
ical Properties and Finished Surface Struc-
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JADA 85:101-108, 1972.
19. BRADEN, M.: Composite Filling Materials,
London: Cottreil and Company.
20. BARTON, J.A.; BURNS, C.L.; CHANDLER,
H.H.; and BOWEN, R.L.: An Experimental
Radiopaque Composite Material, J Dent Res
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21. NIELSEN, L.E.: Mechanical Properties of
Polymers, New York: Reinhold Publishing
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(methylmethacrylate), Modern Plastics 32: 25. HARTMANN, B. and JARZYNSKI, J.:

138, 1955.
23. BEECH, D.R. and BROWN, D.: The Role of
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24. BRADEN, M.: The Absorption of Water by
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1968.

INTERNATIONAL SYMPOSIUM
on
"Oral Immunogenetics and Tissue Transplantation"
At UCLA
March 12 and 13, 1981
to be held in
The Neuropsychiatric Institute Auditorium
Center for the Health Sciences
UCLA

This Symposium will include review papers on the immunogenetics of mouse, rabbit,
rhesus monkey and man, as well as research papers on a wide variety of related subjects
given by distinguished scientists from the United States, Scandinavia, Scotland,
England, Australia, and New Zealand. The Proceedings will be published as a separate
monograph by Elsevier-North Holland.
Inquiries may be addressed to: Dr. George Riviere or Dr. William Hildemann
(Conference Co-chairmen), Dental Research Institute, UCLA School of Dentistry,
Los Angeles, CA 90024.

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