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Philip S.

Baker, DDS
Assistant Professor
Arthur E. Clark, r, PhD. DMD
Professor and Chairman

Compositional Influence
on the Strength of
Dental Porcelain

Department of Prosthodontics
College of Dentistry
University of Florida

This work compared the tensile strength of two glass


compositions with published values of currently available
dental porcelains. The influence of several variables, such as
air and vacuum firing, firing temperature, surface roughness,
immersion in water, and the inclusion of filler particles, on
the inherent strength of the glass compositions is also
discussed. The authors developed a glass frit having a tensile
strength of 102.4 MPa as determined by the biaxial flexure
technique. This value compares favorably with the reported
strength of commercial brands of feldspathic porcelains. The
strength of this glass was not significantly reduced as a result
of surface abrasion or immersion in distilled water. Int I
Prosthodont 1993:6:291-297.

ceramics are generally recognized as beD ental


ing esthetically superior to other restorative

the thinness of the strengthened layer and the


deleterious effects of scratches on treated surfaces.
dental materials. They exhibit excellent tissue comPenetration or scoring of the layer can result in a
dramatic weakening." Hence, further investigation
palibility, extreme chemical durability, and low
into alternative strengthening methods is warthermal conductivity. Unfortunately, dental ceranted.
ramics are fragile and can fail when exposed to
masticatory stresses. This results from their brittleAnother method to improve the mechanical
properties of dentai porcelain is bulk strengthenness as weli as their low tensile and shear strength.
ing, ie, producing a porcelain with a uniform inNumerous investigators have attempted to evaluate
crease in strength. Dental porcelains are basically
and improve the strength of dental ceramics with
aluminosilicate glasses with residual quartz crystals
varying degrees of success.'"" These techniques
and a small percentage of pigmenting agents. In a
fiave included modification of current products as
composite system with a continuous glass matrix,
well as development of new materials to attempt to
crystalline dispersions limit the size of the Griffith
replace porcelain.
flaws and strengthen the system.''For crystals to act
One approach toward strengthening dental poras effective strengthening agents, however, they
celain involves an ion exchange technique. If a
should possess a thermal expansion similar to the
large ion replaces a smaller one, compressive stress
matrix phase to prevent the introduction of stress at
is produced in the exchanged region. A number of
the matrix-crystal interface. In dental porcelains the
studies on strengthening dentai porcelain by using
cooling shrinkage of quartz inversion at 573^ can
ion exchange have been reported,' ' and all dembe so great that the quartz particles separate from
onstrated a significant increase in the modulus of
the glass matrix. McLean and Hughes' reported on
rupture. Potential limitations to this technique are
replacing the quartz crystalline phase with alumina
and observed a significant improvement in
strength. This resulted in part from the lower exReprint requests: Dr Philip S. Baker, Department of Prosthodon- pansion of alumina particles which enabled them to
remain in intimate contact with the glass matrix.
tics, College of Dentistry, Unn/ersity of florida. Box W045,
Gainesville, Florida 32610-0435.

6, Number 3,1993

291

The [nternatiorai loutnal of Prosltiodontii

Compositional Inlluence on Dentai Potceiain

Unfortunately, although alumina particles


strengthen porcelain, they also increase its opacity,
Southan' has classified modern dental porcelains
into two groups: one group having an intact vitreous matrix and the other having a disrupted vitreous matrix. The first group includes aluminous porcelains and any feldspathic porcelains having
matrices that are sufficiently plastic at 573''C to
accommodate the volumetric shrinkage of the
quartz inversion. The second group includes feldspathic porcelains having matrices that are rigid at
573^, When porcelains in this group are cooled,
the glass matrix is stressed to the point where
microcracks are formed, Southan's data indicated
that aluminous porcelains were not significantly
stronger than matrix-intact feldspaf hie porcelains.
The implication of this concept is that strengthening may be achieved with quartz filler particles if
the viscosity or rigidity of the glass matrix is such
that the volumetric contraction of the quartz particles does not set up stresses at the quartz-glass
interface.
Although the presence of crystals, whether
quartz or alumina, can strengthen a dental porcelain under proper conditions, fracture may also
propagate through the glass in the regions between
crystalline particles. Therefore, an inquiry into
methods of strengthening the glass matrix is warranted.
The purpose of this study was to measure the
tensile strength of two glass compositions developed by the authors and to compare these materials with currently available dental porcelains. The
influence of firing temperature, surface roughness,
water immersion, and inclusion of filler particles on
the new glasses was also evaluated.

Fig 1 Diagram of biaxial fiexure test device.

Instrument Corp, Hightstown, N|) with an accuracy


of 0.1 g. The mixtures were melted in platinum
crucibles in a temperature range from 1,300C to
1,450''C for 24 hours in a high-temperature ceramic
furnace (Model LCH, Burrell Corp, Pittsburgh, PA).
The molten glass was quenched once in water producing the frit. The fritted materials were ball
milled using a jar mill (US Stoneware, Akron, OH)
and pelleted milling medium (Burundum Grinding
Medium, Fisher Scientific) and sieved to -100 and
-325 mesh powders. No colorants were added.
Discs were prepared by dry powder compaction of
4 g of powder in 28.6-mm-diameter dies {Fred S.
Carver, Inc, Menomonee Falls, W!), An applied
load of 103.4 MPa was used (Carver Laboratory
Press, Fred S. Carver, lnc. Pressed specimens were
fired in sets of 10 in a porcelain oven (Jelenko TruFire VPF, elenko Dental Health Products, Armonk,
NY) by gradual introduction into the oven muffle at
600^C and firing to final temperatures at a heating
rate of 50C per minute. The discs were fired for 1
hour at the final temperatures, then air cooled to
room temperature (22.5X] on the firing tray placed
upon the porcelain oven stage.
Three groups of samples were fired. Croup 1
consisted of 50 samples of composition L-1 and
10 samples of 80% L-1 combined with 20% AkO,,
fired under different conditions, with selected
samples then being air abraded (Abrasive Blaster,
50-|j.m aluminum oxide. Belle de St Claire,
Chatsworth, CA) while others were immersed in
distilled water for 24 hours; group 2 consisted of
samples of composition L-1 sieved to two different
particle sizes; and group 3 consisted of 10 samples
of composition A-2 and 10 samples of 60% A-2
combined with 40% A1,O.

Materials and Methods


The glasses were prepared from reagent grade
sodium carbonate, calcium carbonate, potassium
carbonate, boric anhydride, aluminum oxide
(Fisher Scientific, Pittsburgh, PA), and S-jxm silica
(Min-U-Sil 5|j,m, Pennsylvania Class Sand Corp,
Pittsburgh, PA). The two glass compositions reported in this paper are:
1, L-1, composed of 65% SiO,, 5% AljO,, 4% K,0,
16% Na,0,10% CaO, and Q% B,0,
2. A-2, composed of 40% SiO,, 30% AI^Oj, 2% K,0,
8% Na,0,10% CaO, and 10% B,0,
The authors formulated 200-g batches of each
composition by weight using an electronic balance
(Mettler Flectronic Balance Model BB 240, Mettler

The internationai Joumai of Protiiodontics

292

Volume 6,

Compositional Iniluenceon Denial Porcelain

Fig 2 Mean tensiie breaking


stress measures for six series ot
sampies ot composition L-1.

Comp L-1
A Air Fired 700C 1 h
B Air Fired 75O'C 1 h
C Air Fired 700^C 1 h
Surface Abraded
D Vacuum Fired 700C 1 h
E 80% L-1 + 20% AljC,
Air Fired/oO'C 1 h
F Air Fired 70DC 1 h
immersed

140
120
100
80
60
40
20
0
Sample Series

Samples were then subject to mechanical stress


via the biaxial flexure method developed by Wachtman et al." This method entails use of a thin circular disc placed on three equally spaced ball bearings with the specimen loaded at tbe center of the
support circle (Figi).
The apparatus was placed in a universal testing
machine (Instron Model 1125, Instron Corp, Canton, MA) and loaded at a rate of 1.27 mm/min. The
tensile stress developed in the center of the lower
surface of the plate can be calculated as follows."

3P

II]

Hughes' have made use of a related technique and


noted a similarity to stresses that are likely to occur
in a thin section such as a jacket crown.

Results
Figure 2 presents the mean tensile breaking
stressforthe tests of composition L-1 (group 1]. Six
conditions were tested and the results of each condition represent the average of ten samples. The
powder size for all six series was - 325 mesh or iess
than 44 |i.m. The mean tensile strength for composition L-1 when air fired at 700C for 1 hour and air
cooled is 86.8 13.2 MPa (series A). Raising the
firing temperature SOX resulted in a mean breaking stress of 102.4 16.0 MPa (series B]. Series C
represents the mean strength of composition L-1
when fired at 700C and surface abraded prior to
mechanical testing. The mean breaking stress was
81.6 18.5MPa. When vacuum fired for 1 hour, the
mean flexure strength of composition L-1 was 77.5
19.6 MPa (Series D]. Series E shows the mean
flexure strength for a mixture of 80 wt% L-1 powder
and 20 wt% ALO,. When air fired for 1 hour at 75O''C
the mean was 102.8 17.0 MPa. A series of L-1
samples was air fired at 700C for 1 hour and then
immersed in distilled water for 24 hours prior to
mechanical testing series F]. The mean breaking
stress was 88.7 27.4 MPa.

(XY)

where
12]

^ ^ (1 - [TD

(3)
where |v] = Poisson's ratio, = radius of loaded
area, A = radius of support circle, C = radius of
specimen, P = applied load, and D = thickness.
An advantage of this test is that slightly warped
specimens may be used without affecting the
results. The effects of edge flaws seen with rectangular bar specimens are minimized." McLean and

ume 5, Number 3,1993

293

Compositional Inllucrceon Dental Porcelain


Table 1

One-way ANOVA Resulfs


Group 1
Between
groups

Source
DF
SS
MS
F
P

Table 2

Group 2

Within
groups

Total

54

59

5563.4
111268
3 04

19767,69
366,07

25331.09

<05

Between
groups

Total

36

39

4024.3
1341.43
3,75
<.O5

12893.85
358.16

16916.15

7518.2
2506.07
10.43
<.O1

Unpaired ! Test Results

Sample series

Mean"

SD

Group 1 E
8
F
A

i02.e

17.0
16.0
27.4
13.2
18.5
19.6

c
D

102.4
88.7
86.8
81.6
77.5

Group 2 C
A
B
D
Group 3 D
C
B
A

100.9
86.8
77.5
75.5
102.8
102.4
75.9
74.5

Group 3

Within
groups

24.2
13,2
19.6
16.7
17.0
16.0
9,6
1S.0

"Values connected by vertical lines are nol statistically different [P < 05)

Significant intragroup hreaking strength differences were identified for composition L-1 by oneway analysis ot variance (Tahle 1) and unpaired (test
(Table 2) and revealed the following: (1 sample
series B and E were statistically similar, buf were
significantly different trom series A, C, D, and F (P
< .05); and (2] sample series A, C, D, and F were
statistically similar in mean breaking sfrengfh.
Figure 3 shows a comparison of fhe mean flexure
strength for two different particle size ranges of M
for air-fired and vacuum-fired conditions (group 2).
For the -325 mesh L-1 powder the air-fired breaking sfrength was 86.8 13.2 MPa (series A) and the
vacuum-fired value was 77.5 19.6 MPa series B).
For fhe -100 mesh |< 150 |i,m) L-1 powder the airfired breaking stress was 100.9 24.4 MPa (series
C) and fhe vacuum-fired value was 75.5 16.7 MPa
(series D].
ANOVA revealed significanf differences between
the group 2 sample series of varied particle sizes
(Table 1). The results of tests (Table 2) indicated
that sample series A, B,and D were not significantly
different; but A, B, and D significanfly differed
from series C[P< ,05).

The Internaiional lournal of Prosthodontics

294

Between
groups

Within
groups
36
8650.44
240.29

Total
39
16168.64

Figure 4 presents the mean flexure stress for


composition A-2, which contains 40 wt% silica an
30 wt% alumina (group 3, series A). When air fired
for 1 hour at 800X, the mean value was 74.5 18.0
MPa (Fig 4, series A). A mixture of 60 wt% A-2 frit
plus 40 wt% ALO, (group 3, series B), fired at 1,000"
C for 1 hour, had a mean breaking strength of 75.9
9.6 MPa (Fig 4, series B). The mean breaking
sfrengths of composition L-1 air fired at 750C
(group 1, series B) and the mixture of L-1 plus 20
wt% alumina air fired at 750C (group!, series E)are
also included in Fig 4 for comparison and, for this
figure only, are labeled series C and D,
Statistical analysis by one-way ANOVA (Table 1)
and unpaired t test (Table 2) for compositions A-2
(group 3, series A) and A-2 plus h\,O (group 3,
series B) disclosed no significant difference befween series A and B, but a significant difference
did exist between the A-2 compositions (series A
and B) and the group 1 L-1 compositions included
for comparison [P < ,05).
Discussion
Becauseof the uncertainties of comparing tensile
properties of glasses determined by different testing techniques,'" the data in this work are compared with the data presented by McLean and
Hughes' since their method was similar to that of
the present study. It consisted of placing 1-mmthick porcelain, porcelain and alumina, or alumina
discs on a lead foil washer against a circular knife
edge and loading the discs from the opposite side
with a hardened steel ball at a rate of 104 kg/min.
Although there are few data of this type in the
literature, it is feif that the features associated with
the biaxial flexure technique as discussed earlier
simulate the conditions of mechanical stressing encountered in a clinical situation.' McLean and
Hughes reported the average breaking strength of
a medium-fusing air-fired porcelain as 60.5 MPa, a
medium-fusing vacuum-fired porcelain as 66.5
MPa, and a low-fusing air-fired porcelain as 66.5

Cumpositiorai Influence on Dental Porceii


Fig 3 Mean flexure stress measures for two particie size ranges
of air- and vacuum-tired composition L-1,

Comp L-1
A Air Fired 700C 1 h
-325 Mesh Frit
B Vacuum Fired 700C 11n
-325 Mesh Frit
C Air Fired 700C 1 h
-100 Mesh Frit
D Vacuum Fired 700C 1 h
-100 Mesh Frrf

140 r
120
100
80

60
40
20

Sample Series

Fig 4 Mean fiexure stress measures tcr compositions A-2, A-2


pius 40% A I A . L-1. ahd L-1 plus
20% ALO,.

A Comp A-2 Air Fired


aooc 1 h
B 60% A-2 + 40% AljO
Air Fired 1000C 1 h
C Comp L-1 Air Fired
750^ 1 h
D 80% L-1 + 20%Ai;O3
Air Fired 75QC 1 h

140
120
'S
%.
S
w

""^
80
60
40
20
O
Sample Series

Vacuum firing glass L-1 at 700C led to a mean


flexure strength of 77,5 MPa and a rather large
coefficient of variation of 25%, Microscopic examination of fractured specimens of glass L-1 which
had been air fired and vacuum fired indicated that
the vacuum-fired specimens contained larger
pores than the air-fired samples. The presence of
these defects could account for the greater data
dispersion of the specimens fired under vacuum.
Immersion of specimens of glass L-1 in distilled
water (Fig 2, series F) 24 hours prior to mechanical
testing did not produce any notable weakening

MPa. The average breaking strength for composition L-1 was 86,8 MPa when air fired at 700C and air
cooled (Fig2, series A), The mean breaking strength
of series C in Fig 2 (81,6 MPa) indicates that the
strength of series A is not associated with the formation of a surface compressive layer during the
rapid air cooling period. This is in agreement with
the findings of Corbitt et al,-' in that the strength of
dental porcelain seems more dependent upon infernal configuration than surface flaws. However,
the coefficient of variation did increase from 15,2%
to 22,7%.

re6, Nurrber3,1

295

The International lour

effect (86.8 MPa mean not immersed vs 88.7 MPa


mean immersed). However, longer periods of immersion may lower the tensile strength of dental
porcelains by reducing the energy required for
propagation at the crack tips of surface flaws.- This
effect, termed static fatigue, would not be anticipated after the brief exposure to water in this investigation.
Microscopic examination of the L-1 glass fired at
7(iOC revealed that the particles were still evident
after firing. Incomplete sintering at the boundaries
would produce a situation in which stress transfer
between particles would not be possible. Interestingly, air firing glass L-1 at 700^ with two particle
size ranges produced a mean strength change from
86.8 MPa for the smaller size to 100.943 MPa for the
glass containing the larger particles. However, vacuum firing at 700C produced very similar means for
both particle size ranges. Large voids were present
in the vacuum-fired specimens of both particle size
ranges. Their presence could explain the similar
strengths and rather large coefficients of variation
in each (22% and 25%). If the 700G air-firing temperature does lead to incomplete sintering and
failure at the particle boundaries, then the increased strength observed with the L-1 glass containing larger particles may be attributed to the
presence of fewer potential faiiure sites and indicates that the material should be fired at higher
temperatures. Raising the firing temperature of
glass L-1 from ZOOT to 750T increased the mean
flexure strength from 86.8 to 102.4 MPa. This increase is probably associated with more complete
fusion of the glass particles during sintering.
Series F in Fig 2 shows that the addition of20wt%
alumina to the L-1 glass frit had no effect on the
mean breaking strength. This may be attributed to
the low firing temperature (750G), resulting in incomplete sintering between the glass particles and
the alumina particles. Firing at temperatures near
1,000G to enhance sintering would be impractical
with glass L-1 because of extreme softening of the
glassy matrix.
Binns-' listed the compositions of several commercial dental porcelains. The alkali (Na.O and
K.O) concentration of glass L-1 is 20%, whereas the
commercial brands contain approximately 12%.
The difference was usually replaced by B^O^ additions. The extra alkali content of L-1 should have the
effect of reducing the viscosity at a given temperature." At the onset of this study it was felt that
increasing the alkali content to reduce viscosity
would lower the strength concurrently. The fact
that the strength as determined in this study seems
equal or superior to commercially available porce-

The Internationa

I ot Proslhodonlics

296

lains is most encouraging to further research. Evaluation of larger sample groups with different test
parameters, as well as an examination of the effects
of colorants on the breaking strength of the new
porcelains, should provide information on the feasibility of such compositions for commercial use.
Composition A-2 contains only 40 wt% silica and
30 wt% alumina. Its mean breaking strength when
fired at 800X for 1 hour was significantly iower than
that of glass L-1 fired at 75O'G (74.5 MPa vs 102.4
MPa). As with glass L-1, the incorporation of alumina particles with the glass frit had no significant
effect on the mean hreaking stress. However, the
coefficient of variation was reduced from 26% to
14%. It should be noted that Jones and Wilson"
found that the inclusion of small amounts of alumina (5% to 20%) to veneer porcelains did not act as
an effective strengthening phase.
Conclusions
A glass frit has been developed which has a tensile strength of 102.4 MPa as determined by the
biaxial flexure technique. This value compares favorably with the reported strength of commercial
brands of feldspathic porcelains. The results of this
study suggest the foliowing conclusions.
1. Air firing glass composition L-1 at 75O''C produced a significantly stronger porcelain than
firing itat700C.
2. The addition of 20 wt% A[,0, to composition L-1
air fired at 750G had no significant effect on
breaking strength.
3. When fired at700C, no significant difference in
breaking strength was noted for conditions of
air firing, vacuum firing, air abrasion, or shortterm water immersion for glass composition L-1.
4. Air-fired -100 mesh particle size glass L-1 was
significantly stronger Ihan vacuum-fired -100
mesh, or air-or vacuum-fired -325 mesh size at
the 700C firing temperature.
5. Glass compositions L-1 and 80% L-1 plus 20%
AljOj, fired at 7.WC, were significantly stronger
than glass A-2 (40% silica and 30% Al ,Oj) air fired
at 800C, or 60% A-2 plus 40% alumina particles
fired at1,000C.
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297

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