Study of the physical properties of type IV gypsum, resin-containing, and

epoxy die materials

Philip Duke, DDS, MSD,a B. Keith Moore, PhD,b Steven P. Haug, DDS, MSD,c and Carl J. Andres, DDS,
MSDd
Indiana University School of Dentistry, Indianapolis, Ind.
Statement of problem. Little published information is available comparing the properties of recently
developed resin-modified gypsum and epoxy resin die materials, which are claimed to be superior to conventional type IV gypsum die materials.
Purpose. This study compared the properties of 3 new die materials and 2 conventional type IV gypsum
products.
Methods and material. The linear dimensional change, detail reproduction, surface hardness, abrasion
resistance, and transverse strength of 2 recently introduced, resin-modified gypsum die materials (Resinrock
and Milestone), a new epoxy resin die material (Epoxy-Die), and 2 conventional type IV gypsum die materials (Silky-Rock and Die-Stone) were studied.
Results. All gypsum products expanded, whereas the epoxy resin material contracted during setting. The
epoxy resin exhibited much better detail reproduction, abrasion resistance, and transverse strength than the
gypsum materials, which were similar in these properties. A conventional type IV gypsum exhibited the
highest surface hardness, whereas the epoxy resin had the lowest value.
Conclusion. The resin-modified gypsum products were not significantly superior to the conventional
type IV gypsum die materials. In general, the epoxy resin exhibited the best properties of the materials studied; however, its setting shrinkage may necessitate alterations in technique to achieve well-adapted castings.
(J Prosthet Dent 2000;83:466-73.)

CLINICAL IMPLICATIONS
Of the die materials studied, only the epoxy resin exhibited several physical properties
that may be superior from a clinical point of view. However, its setting shrinkage compared with the expansion observed with gypsum die materials may require modifications in technique to obtain castings that will be well adapted to the tooth preparation.
The properties of the 2 resin-modified gypsum materials were not significantly different from those of the 2 conventional type IV gypsum products included in this study.

ince the advent of elastomeric impression materials,

the use of indirect techniques for fabrication of
prosthodontic restorations has become almost universal. Success of these techniques is dependent on the
availability of a die material that meets certain clinical
criteria. Type IV gypsum products that meet the American Dental Association (ADA) Specification No. 251
are most commonly used as die materials.
Although these have been successfully used for many
years, numerous attempts have been made to develop a
die material with improved properties.2,3 Specific areas
of interest have included improved strength,4,5
improved resistance to brittle fracture,6-8 improved surface hardness,9-11 abrasion resistance,12-14 improved

accuracy,15-19 and detailed reproduction.20-24 Die

stones with improved strength have been marketed as
type V materials, and the use of resin die materials25,26
and resin coatings on gypsum dies27,28 has been investigated.
This study investigates 2 new commercial, resinreinforced gypsum products and a new epoxy die material. Each of these is claimed to have improved properties compared with conventional type IV gypsum die
materials or to resin die materials previously marketed.
The purpose of this study was to compare a broad cross
section of physical properties of these new materials
with 2 type IV gypsum products that meet ADA Specification No. 25.

MATERIAL AND METHODS

aAssistant

Professor of Prosthodontics.
bProfessor of Dental Materials.
cAssociate Professor of Prosthodontics.
dProfessor of Prosthodontics.
466 THE JOURNAL OF PROSTHETIC DENTISTRY

Included in this study were 2 newly marketed resinreinforced gypsum die materials, Resinrock and Milestone, a new epoxy resin die material, Epoxy-Die, and
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Table I. List of die materials tested and mixing proportions

Die material

Manufacturer

Water/powder
ratio*

Mixing times
(seconds)

Silky-Rock (type IV)

Whip Mix Co, Louisville, KY

23/100

30

Die-Stone (type IV)

Modern Materials, Heracus Kulzer Inc,

South Bend, IN

22/100

15

Resinrock (resin
containing type IV)

Whip Mix Co, Louisville, KY

20/100

30

Milestone (resin
containing type IV)
Epoxy-Die (epoxy
resin die material)

Modern Materials, South Bend, IN

20/100

15

B/A ratio (mL of base

per mL of activator)
5/0.83

30

Ivoclar, North America Inc,

Amherst, NY

Batch no.

Packaged in
envelopes of 70 g
each, 028598005
Packaged in a 25-lb
bag, 9712091
Packaged in
envelopes of 70 g
each, 105497002
Packaged in a 25-lb
bag, 9711006
Assortment kit, 912832

*Milliliters of water per 100 g powder.

Gypsum-based products.

2 conventional type IV gypsum die materials, SilkyRock and Die-Stone (Table I). The properties investigated included: linear dimensional change, detail
reproduction, surface hardness (Knoop), transverse
strength, and abrasion resistance with dull and sharp
abraders. These properties were chosen because it was
believed that they have the greatest practical significance in the use of die materials.
Specimen preparation and all tests were performed
at room temperature (23C 2C) and approximately
50% relative humidity. Five specimens for each material
were prepared and used for dimensional change, detail
reproduction, and hardness measurements. Five additional specimens per material were prepared for abrasion testing. Twice as many specimens per material
were prepared for the transverse strength test because
of the possibility of obtaining results with considerable
standard deviations due to the haphazard effect of
internal porosity.4
Impressions of a rectangular stainless steel master
die, 6 6 38 mm (Fig. 1) were made using a low-viscosity polyvinyl siloxane impression material (Examix,
GC America, Alsip, Ill.), in light-cured resin custom
trays (Triad Trutray, Dentsply International, York, Pa.).
All impressions were subjected to a simulated infection
control process by spraying with a phenolic surface disinfectant, Pro Spray (Cottrell Ltd, Englewood, Colo.).
The sprayed impression was placed in a closed plastic
bag for 15 minutes, then thoroughly rinsed and dried
before pouring with die material.
Gypsum die materials were proportioned (Table I)
and mixed with deionized water at the ratios shown.
Materials were hand mixed in a 200-mL Vac-u-Mixer
bowl (Whip Mix Corp, Louisville, Ky.) until the powder was wetted and then mechanically mixed under vacAPRIL 2000

uum at 400 rpm in a Vac-U-Vestor (Whip Mix). Two

impressions were poured with each mix. Gypsum specimens were separated from their impressions 1-hour
after mixing.
A total of 25 impressions were made. Each impression was poured a total of 4 times. The first time the
impressions were poured to obtain the specimens used
for the dimensional change, detail reproduction, and
hardness tests, properties that required an original
impression. The second time the impressions were
poured to obtain the specimens used for abrasion resistance tests, and the third and fourth times to obtain
specimens for the transverse strength test. To test these
2 properties, the same molds were used because specimens were reshaped after being retrieved from the
mold before testing. Different die materials were not
poured into the same impression because of the risk of
contaminating materials with one another.
The base/activator ratio used for the epoxy die
material is presented in Table I. Before mixing the
epoxy, the silicone impression surface was brushed with
the wetting powder provided in the kit and then compressed air was used to blow out excess powder. Five
milliliters of base were mixed with 0.83 mL of activator
by hand in a plastic cup for 30 seconds.
Before the mixed epoxy was poured, the inner surfaces of the impressions were coated with a thin layer
of epoxy by using a small brush. The isolating liquid
supplied with the epoxy material was not used because
no difficulties were found when separating the dies
from their impressions. In a pilot experiment, the use
of the isolating liquid appeared to reduce the detail
reproduction of the epoxy die material. Epoxy specimens were separated from their impressions 3 hours
after mixing.
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DUKE ET AL

Fig. 1. Stainless steel master die mounted on indexing base,

custom resin impression tray, and addition silicone impression.

Linear dimensional change

The large crossed Knoop indentations at either end
of the master die defined the reference distance for
dimensional change determination (34 mm) (Fig. 2).
The silicone impressions were stored for at least 2
weeks to allow the dimensions of the tray and impression materials to stabilize. The reference distance on
the impression was measured 5 times with a Nikon
measuring microscope (UM-2, Nikon, Garden City,
N.Y.) at 100 to a resolution of 1.0 m. An average
of the 5 measurements was calculated.
Five dies were poured for each die material. Twentyfour hours after the dies were poured, the reference distance was measured on each die as it was measured on its
respective impression. The difference in values for the
die and its impression were used to calculate a percentage change in length. The average and standard deviation of 5 specimens for each material was calculated.

Detail reproduction
The 15 engraved lines of varying widths on the master dies were used for detail reproduction evaluation
(Fig. 2). Every impression used replicated all these
lines. Dies were examined at 25 magnification with
low-angle lighting to determine the narrowest line seen
in each die. At least 90% of the line needed to be replicated to count it as present.

Knoop hardness
Knoop indentations were made on the lateral surfaces of the dies. Five indentations, 5 mm apart, were
made on each die with a Leco M-400 hardness tester
(Leco Corp, St Joseph, Mich.) with a Knoop indenter
and a 500-g load applied for 20 seconds. The average
of the 5 readings for each specimen was used to calcu468

Fig. 2. Schematic view of upper surface of master die shows

test groves used for detail reproduction and Knoop indentations used to define reference length.

late a group mean and standard deviation for the 5

specimens of each die material.

Abrasion resistance to sharp and dull abraders

Five specimens were poured with each die material
and the dies were stored for 24 hours before testing.
The abrasion apparatus is depicted in Figure 3. The
apparatus moves the abrader in a reciprocating motion
at 284 mm/min over a 20-mm stroke. Specimens are
supported in a V-block holder, so that a long line angle
of the specimen is held in a vertical position for abrasion. The 2 line angles formed at the bottom of the
impression were used, one for each type of test. Two
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Fig. 3. Reciprocating abrader apparatus.

abraders were used: sharp, a utility knife blade, and

dull, a 0.020-in. round stainless steel orthodontic wire.
These were mounted in a hinged metal holder that provided an abrasion load of 0.42 N (Fig. 4).
Each specimen was subjected to a complete abrasion
cycle (forward and reverse stroke) using the sharp
abrader to define an initial surface width on the specimen. The specimen was removed from the apparatus
and the initial width measured at 20 at 5, 10, and
15 mm from the end of the specimen to determine an
average initial width. Specimens were returned to the
apparatus and abraded for 75 complete cycles with
either the dull or sharp abrader. The average width after
abrasion was measured for each specimen. Widths
before and after abrasion were used to calculate an
abrasion volume loss for the specimen. Means and
standard deviations for each group were calculated
from the volume loss for each of 5 specimens.

Transverse strength
Ten specimens were prepared for each die material
and stored for 48 hours before testing. The irregular
free surface of each specimen was ground flat and parallel to the opposite surface and finished with 600-grit
SiC paper. The finished width and thickness of each
specimen were measured with a digital micrometer.
The specimens were tested with a 3-point loading
apparatus in a universal testing machine (Sintech 1123
Renew, Minneapolis, Minn.) to failure at a crosshead
speed of 0.1 mm/min. The ground side of each specimen was positioned so that it was in compression
during the test. The span length used in the test was
20 mm. Load at fracture was used to compute transverse breaking strength in MPa. Means and standard
deviations for the breaking strength were calculated
from the 10 specimens in each group.
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Fig. 4. Close-up of slotted abrader holder and hinged mounting rod (top) shown with brass tube photo-holding 0.020-on.
orthodontic wire (dull abrader). Brass tube assembly was substituted for utility knife blade to form sharp blade (bottom).

Statistical analysis
One-way analysis of variance (ANOVA) was performed on the means and standard deviations for the
groups for each test. Newman-Keuls multiple comparisons were then conducted to test for statistically significant differences between specific materials for each
property. A significance level of P<.05 was used in all
statistical analyses.

RESULTS
Linear dimensional change and detail
reproduction
ANOVA indicated a significant difference among
the groups (Fig. 5). Newman-Keuls multiple comparisons indicated that the gypsum die materials were not
significantly different among themselves but did differ
significantly from the epoxy die material. Expansion
was seen with all gypsum materials, whereas the epoxy
exhibited a comparable amount of contraction. The
narrowest lines reproduced in the dies of each material
are shown in Table II. The limit of reproduction for the

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DUKE ET AL

Fig. 5. Percentage linear dimensional change of die materials. Positive values represent setting expansion and negative
values contraction. Groups identified by same letter are not
significantly different.

Fig. 7. Volume loss after 75 cycles with dull and sharp

abraders. Groups identified by same letter are not significantly different.

Table II. Detail reproduction of the 5 specimens tested*

Die material

Epoxy-Die
Silky-Rock
Die-Stone
Resinrock
Milestone

Line width (m)

1
17
17
17
17

1
17
17
17
17

1
17
17
17
17

1
17
17
17
17

1
17
17
17
17

*Narrowest line reproduced. N=5. If 90% of the line was visible at 25 magnification, the line was classified as reproduced.

Fig. 6. Knoop hardness of die materials. Groups identified by

same letter are not significantly different.

gypsum materials was 17 m, whereas the epoxy consistently reproduced the 1-m line.

Hardness and abrasion resistance

Knoop hardness values at 24 hours are shown in Figure 6. ANOVA indicated a significant difference among
the groups and the multiple comparisons showed that
all pairs were significantly different, with the exception
of Silky-Rock and Milestone. Die-Stone had the highest Knoop hardness and Epoxy-Die the lowest.
Volume loss in the tests with dull and sharp abraders
is illustrated in Figure 7. One-way ANOVAs indicated
significant differences among materials in both tests.
Newman-Keuls comparisons showed Epoxy-Die to be
significantly more resistant to abrasion than all other
470

materials. There were no differences between any of

the gypsum materials in the sharp abrasion test, whereas the gypsum products separated into 3 overlapping
pairs in the dull abrasion test. Milestone had the lowest
resistance to abrasion in both tests. The sharp abrasion
test produced 12 to 76 times more wear than the dull
test. The rank order of materials in the 2 tests was nearly identical.

Transverse strength
Transverse strength values are depicted in Figure 8.
ANOVA indicated a significant difference among the
groups. Newman-Keuls comparisons indicated that the
epoxy resin die material was significantly stronger than
the gypsum die materials that did not show significant
differences between them. Transverse strength of the
epoxy resin was more than 3 times greater than the
gypsum products. All gypsum materials exhibited britVOLUME 83 NUMBER 4

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Fig. 8. Transverse strength of die materials. Groups identified

by same letter are not significantly different.

Fig. 9. Representative load-deflection curves in transverse

bending for die materials.

tle fracture at very low deformation, whereas the epoxy

showed an extended range of elastic deformation
before fracture as shown in Figure 9.

epoxy die that is 0.16% smaller could lead to a clinically unacceptable casting that would not seat on the prepared tooth unless compensatory laboratory techniques
are introduced.19 If the epoxy is compared with a typical type V high-strength gypsum die material, this discrepancy is even larger.
Sources of error related to impression and tray material dimensional changes were minimized by storing the
molds until they had stabilized. Influence of the thermal coefficient of expansion of the addition silicone was
also minimized by conducting the experiment at relatively controlled room temperature and humidity. All
measurements were made by the same investigator and
reproducibility of the measurements between reference
marks was better than 1.5 m or 0.01% of the total
distance. Unlike the testing methodology of ADA
Specification No. 25, which uses a 90-degree, V-shaped
ruled trough, the method used in this study did
not allow for unrestricted initial expansion. This was
performed in an attempt to better simulate clinical
conditions.

DISCUSSION
Linear dimensional change
The results of this study are in agreement with those
of previous studies15-17 that reported a setting expansion of type IV dental stones below 0.1%. These values
are in accordance with the requirements for setting
expansion in ADA Specification No. 25. The setting
expansion data printed on the packages of the gypsumbased materials are as follows: Silky-Rock, 0.09%; DieStone, 0.07%; Resinrock, 0.08%; and Milestone, 0.08%,
which are in reasonable agreement with the results of
this study.
The water-powder ratios used to mix the resin-modified gypsum materials, Resinrock and Milestone, were
lower than those used for conventional gypsum die
materials, Silky-Rock and Die-Stone. The results
showed that the former materials expanded slightly less.
Although lower water-powder ratios tend to increase
setting expansion of gypsum products,18 the addition
of resin lowers the total gypsum content, which may
explain the reduced expansion. In addition, polymerization shrinkage of the epoxy resin was greater than
that claimed by the manufacturer (0.05%), and slightly larger than the average setting expansion of the
gypsum-based materials. Values reported by another
study15 that tested epoxy resin die materials are similar
to those found in our study.
The contraction of the epoxy resin die material
Epoxy-Die may be of clinical significance. If the indirect technique has been optimized to produce welladapted castings by using type IV gypsum products, an
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Detail reproduction
The compatibility between impression materials and
die materials is critical and has been extensively studied.20-22 The die materials tested in this study proved to
be compatible with the impression material used and
easily met the criteria for detail reproduction in the
ADA Specification No. 25.
The results of our study regarding detail reproduction supported those from previous studies23,24 in
which the detail reproduction capabilities of epoxy
resin die materials excelled over those of gypsum-based
materials. The size and irregularities of the gypsum
crystals18,23 preclude gypsum-based products from cap471

THE JOURNAL OF PROSTHETIC DENTISTRY

turing details at the level that epoxy resin die materials

are capable of reproducing. Optical properties of these
materials are another important factor to consider.
Unlike the epoxy resin die material tested, the gypsumbased materials scattered light and required low-angle
illumination to see details. It was evident that not only
were details better reproduced by the epoxy resin die
material, but they also were easier to see.

Hardness
The Knoop hardness test was chosen for this study,
because one of the materials tested was an epoxy resin.
Epoxy resins are known to exhibit elastic recovery after
indentation. Because this elastic recovery occurs mainly along the shorter diagonal of the Knoop indentations, a more accurate measure of the hardness is
obtained from the length of the long diagonal that
exhibits very little elastic recovery.
This study (Fig. 6) reported Knoop hardness values
ranging from 19.8 to 22.4 for the conventional gypsum
products. These values are in relative agreement to
those in another study9 investigating type IV that
found Knoop values of 21.6 for Vel-Mix and SilkyRock. The resin-containing gypsum die materials,
Resinrock and Milestone, were not more resistant to
indentation than Silky-Rock and Die-Stone. The results
of this study also are in agreement with other studies,10,11 which concluded that epoxy resin die materials
are less resistant to indentation than type IV gypsumbased die materials.

Abrasion resistance
The sharp and dull abraders used in this study were
chosen to simulate procedures where sharp and dull
instruments are used. The results of this study agreed
with other studies,12,13 which concluded that the abrasion resistance of epoxy resin die materials was higher
than that of gypsum-based die materials.
As confirmed by other studies,12,14 no correlation
between hardness and abrasion resistance was encountered in our study. The die materials that were the least
resistant to indentation, Epoxy-Die and Resinrock,
were the most resistant to both dull and sharp abrasion.
Conversely Die-Stone, Silky-Rock, and Milestone,
which were the most resistant to indentation, were the
least resistant to abrasion. Hardness may be of limited
value for comparing die materials for clinical use. The
resin-containing die materials, Resinrock and Milestone, performed differently from each other. Among
all the gypsum-based die materials tested, Resinrock
ranked first in its resistance to both sharp and dull abrasion, whereas Milestone ranked last.

Transverse strength
Transverse strength was used in this study because
brittle materials usually fail in bending or tension, not
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DUKE ET AL

compression as used in ADA Specification No. 25. This

study tested the transverse strength of the die materials
48 hours after the specimens were poured. Other studies4,5 have reported dry strength compressive values
of gypsum products, and the values obtained were
approximately twice those of the wet strength tested
1 hour after mixing. Transverse strength is particularly
sensitive to the surface quality of the surface placed in
tension. The specimens were tested with the surface
poured against the impression material in tension so
that grinding and finishing would not influence the
strength values.
The values for the gypsum-based die materials
reported in this study (Fig. 8) do not greatly differ
from one another but are all significantly less than that
of the epoxy die material. The value found in this study
for the resin die material is similar to those of another
study6 of resin die materials that reported values from
82.8 to 91.8 MPa. The results of this study are in
agreement with others,7,8 who have found much higher transverse strength values for epoxy die materials
than those of gypsum-based materials.
All the gypsum-based die materials tested were brittle and exhibited very limited deformation before fracture. The epoxy die material was much less stiff than
the gypsum products and displayed significant elastic
deformation before failure. Comparing the strength
plots in Figure 9, the area under each curve is proportional to the energy required to fracture the material.
Clearly, the epoxy will absorb much more energy
before fracture and should be less susceptible to breakage if dropped or handled roughly.

CONCLUSIONS
Within the limits of this study, the following conclusions were drawn:
1. The properties of the 2 resin-modified gypsum
die materials were not significantly different than those
of 2 conventional type IV gypsum products.
2. The epoxy resin die material was markedly superior in abrasion resistance, detail reproduction, and
transverse strength to all of the gypsum materials
studied.
3. The epoxy resin die material exhibited a setting
shrinkage slightly greater than the average setting
expansion of the gypsum materials. This would likely
necessitate modification in an indirect technique that
has been optimized to produce well-adapted castings
from gypsum dies.
4. Surface hardness does not correlate with the other
properties tested and may not be a good measure of
performance for these materials.
We acknowledge the technical assistance and product support of
Ivoclar-North America Inc, Modern Materials Heraeus Kulzer Inc,
and Whip Mix Corp.
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Reprint requests to:
DR PHILIP DUKE
SCHOOL OF DENTISTRY DS S310
INDIANA UNIVERSITY
1121 W MICHIGAN ST
INDIANAPOLIS, IN 46202
FAX: (317)274-2419
E-MAIL: pduke@iupui.edu

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