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Effect of Firing Temperature and Water Exposure on Crack Propagation in Unglazed Porcelain
K.J. Anusavice and R.B. Lee
J DENT RES 1989 68: 1075
DOI: 10.1177/00220345890680060401
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of
Dental Bionmaterials, College o(f Dentistry, University of Floiida, Gainesville, Florida 32610-0446
Static ftitigue of dental ceramics results from the interaction of residialf tensile stress cand an aqueous environment. 'This phenomenllon is
a potential cause of delayedl crack formation and propagation in ceraimic or metal-ceranmic restorations. For dental ceramics, the influence of microstructural dlejects such as porosity or fissures caused by
incomplete sintering is riot kloown-. 7hle objectives of this study were
to characterize the influence ofporosity (produced by Lindeifirilng) on
the crack propagation resistance of two jeldspathic porcelains (111(d to
determine whether lower stress corrosion susceptibility or higher fractur-e toughness accountss for the superior thermal shock resistance of
0oe of these ceramics.
Wae111
underfired blas oeach porcelain, 25 mmn X 4 mnm X 4 mmt,
by as nutch acs 84C below their recommended firing temperatures.
Atlter polishing the specimens through 0. 05 pm alumina, we induced
cracks in their sum faces wit/i a Vickers mnicrohardness indentert Semicircular cracks, which were produced under an applied indenter load
of 19.6 N, grewt wit/i tine during storage in distilled watem- at 37C.
Underfiring of bat/ ceramics caused a slight increase ini Jracture
toughness and a relatively .small change in pore volume fraction until
we underfired the ceramics at 30'C or more. The crack propagation
data indicate that the higher them-al shock resistance of one of the
ceramics-as measured previously by a water-quench technique-may
be due to its greater resistance to sti-ess cotr-asion at the initial stage
ofcrack proptigation.
Introduction.
The resistance of brittle materials to crack propagation is primarily influenced by surface flaws and microstructural features. Dental ceramics are also susceptible to crack growth
enhanced by moisture. The presence of subcritical tensile stresses
in porcelain due to thermal contraction incompatibility may
cause delayed failure of metal-ceramic restorations. Such residual tensile stresses, even if relatively low in magnitude, may
cause existing flaws to grow with time in the presence of moisture. This reduction in strength, which is caused by a chemical
reaction at crack tips, is known as static fatigue. Jones et al.
(1972) have shown that long-term loading of dental porcelains
at subcritical stress levels will produce failure over periods of
hours or months. Sherrill and O'Brien (1974) have shown that
aluminous and feldspathic porcelains, when tested in water,
exhibit a decrease in flexure strength of approximately 27%.
The presence of porosity in dental porcelain is generally
believed to reduce its strength. However, Jones and Wilson
(1975) have shown that there was no significant difference
between the transverse strength of air-fired porcelains with a
pore volume of 5.6% and vacuum-fired porcelains with a pore
volume of 0.56%. These authors suggested that the predominantly spherical voids found in feldspathic porcelains did not
reduce strength as markedly as did irregularly shaped voids.
Irregular, nonspherical voids might facilitate crack initiation
Received for publication October 23, 1987
Accepted for publication February 16, 1989
This study was supported by NIDR Grant DE06672 and RCDA
DEOO 1 25.
ramics.
1076
-.*- a
No
c0
1077
Vol. 68 No. 6
H = 0.47P/a2
(3)
2n
I( 3n+2
In
c =
(322) In t + I
(3n+)
In[(
in[3n+2
(5)
2
VoXr
Kr(,
(6)
(3n + 2).
Results.
For analyses of fracture toughness, it is essential that the
surface contain no significant residual stresses prior to indentation. If such surface stresses were present, a systematic variation in P/c,,3/2 with load would result. To determine whether
residual stresses were present within the porcelain surfaces, we
initially made plots of P/c03/2 vs. P for each of the two commercial porcelains. The mean values and 95% confidence intervals for each mean for five loads are shown in Fig. 2. As
can be seen in this Fig., the ratio P/c,3'2 was independent of
load. Therefore, we selected the maximum load, 19.6 N, for
all measurements in this study, to minimize measurement inaccuracies associated with smaller cracks.
To ensure that the magnitudes of fracture toughness values
were valid, we made calculations for the soda-lime-silica glass
specimens and compared these values with published values
obtained by conventional test fhethods. Values of K1c and initial crack size are given in Table 1. Data are included for asreceived specimens and for specimens that were polished through
0.05 Am alumina. All specimens had been annealed at 386TC
for 100 h. The 95% confidence interval of the mean and coefficient of variation values are also given. The values of K1c
(Table 1) were in excellent agreement with the value of 0.75
MPa-m 12 reported by Wiederhorn (1969) for soda-lime-silica
glass.
The static fatigue behavior or the relative susceptibility of
the two body porcelains to water-enhanced crack growth in the
presence of residual stress can be determined from plots of log
c vs. log t. Gupta and Jubb (1981) introduced a relatively
simple method for measuring the stress corrosion susceptibility
TABLE 1
Porcelain C
cam
E
Cu
acm
I0
100
to0
0~
Porcelain V
1
I 0,
20
15
10
LOAD (N)
Fig. 2-Load-crack size parameter, P/c,, as a function of load.
25
1078
TIME (sec)
2.3 F
:6
.6
I 07
I
1 I1 1
.4
P=19.6 N
1.2
E
-
n2=0.7
water
.0
CLJ
Cll
en
U
2.2
oil
n=31.5
0.8
0b
cm
CD
0
II
II
6.2
II
6.4
AI
6.6
aI
6.8
7.0
7.2
940
920
900
880
860
840
T (0C)
loads of 17.7 N, 19.6 N, 24.5 N. and 29.4 N. The only apparent difference in the two studies is that we used a higher
aging temperature (37TC) in the present investigation, although
it is possible that differences in the compositions of the sodalime-silica glass specimens may account for this disparity.
Fig. 3 shows that crack growth continued beyond the initial
measurement in the presence of air and paraffin oil for the
annealed glass specimens. The stress corrosion susceptibility
for the three-month period was greater (smaller n value of
20.7) for specimens stored in water than for those stored in oil
(n = 31.5). As-received glass specimens indented in air and
stored in water at 370C exhibited mean crack sizes (c) of 130.7
+ 4.0 pLm, 172.8 + 2.2 plm, 176.6 + 2.1 pm, and 178.8
+ 2.2 Axm at periods of two minutes, one month, two months,
and three months, respectively. Thus, crack growth was negligibly small for the glass specimens during the later period of
aging.
The effect of firing temperature on fracture toughness is
shown in Fig. 4 for each porcelain (nonannealed condition).
The 95% confidence interval is represented by the dotted lines.
The recommended firing temperatures are 971'C for porcelain
C and 920'C for porcelain V. A slight increase in K1c resulted
from a reduction in firing temperature for each porcelain. The
toughness of porcelain C relative to that of porcelain V is
TABLE 2
non-
reduction in firing
temperature.
Vol. 68 No. 6
-10
lbalr
1 10
Porcelain C
P=19.6 N
100
E
0
140 F
_
, -' s
,
,
,,~~~~~~~~
~ ,,
ii
N
01
co
980
11U.
960
940
81 30
130_
L
N
120_
Vo
Porcelain V
-J
:x
900
920
C.)
I1100
Nonannealed
P=19.6 N
150
a n - - _~ ~ ~ ~ ~ - t
901
1079
C.
cc
---..
n=8.9
OF
o0II
920
940
900
LI
880
840
860
T (0C)
Fig. 5-Initial crack size, c,, vs. firing temperature for nonannealed
porcelain specimens.
7;;
90 ,
106
I lI I I I
107
TIME AFTER INDENTATION (sec)
120
V
~~~Porcelain
~~~ <
I,110
~
~ mosI
~ ~ ~ ~ 1
la
P
~~~~~~~~~,
LL
C)
--I~~~~~~~~~~~~~t 2 min
00o
li
90h
H .)..
au,
940
920
900
880
860
T (0C)
840
820
800
Discussion.
Underfiring slightly increased the 'apparent' fracture toughness of the two body porcelains studied, as shown in Fig. 4.
Porosity can affect the calculated value of K1c, in several ways.
First, pores may act to arrest cracks by reducing localized
stress. They can also serve as crack precursors if they are small
or irregular in shape. During the indentation process, pores
may contribute to structural densification and thereby reduce
the driving force for crack growth as the indenter is removed.
One would expect a reduction in the elastic modulus and possibly the hardness with an increase in pore volume (Coble and
Kingery, 1956). Thus, the value of Xr would change and thereby
affect values of Kic. Since the initial size of semicircular cracks
is reduced, an increase in K1c would result. Significant changes
in K1c may not occur until the pore volume increases above a
threshold value, although the effect would vary depending upon
the size and distribution of porosity.
The role of leucite particles in inhibiting crack growth is not
known. Morena et al. (1984) observed that leucite particles do
1080
TABLE 3
STRESS CORROSION SUSCEPTIBILITY COEFFICIENT (n) FOR ANNEALED SPECIMENS AS A FUNCTION OF FIRING TEMPERATURE
Porcelain V
Porcelain C
t = lto3mo
t = lto3mo
to lmo
t< lmo
H20
Oil
T (0C)
Oil
Oil
H20
Oil
T (C)
H20
H20
18.0
12.0
6.8
934
47.0
69.7
38.7
59.0
87.8
985
7.3
107.9
20.4
9.7
920*
48.4
27.5
52.0
55.4
971*
27.3
12.3
63.3
906
63.5
54.7
26.8
5.9
63.8
957
22.2
16.6
59.5
55.9
892
7.0
12.5
50.5
75.1
943
13.4
10.8
24.8
8.8
878
52.2
61.8
78.2
929
75.5
8.5
11.7
864
61.9
92.0
11.6
16.3
51.2
46.4
915
15.5
20.2
58.4
12.0
850
39.8
58.9
47.1
48.0
901
17.4
21.3
9.5
836
62.6
71.2
59.1
49.7
54.0
887
*Recommended firing temperature.
TABLE 4
STRESS CORROSION SUSCEPTIBILITY COEFFICIENT (n) FOR NONANNEALED SPECIMENS AGED IN WATER AT 370C
Porcelain V
Porcelain C
T (C)
t < 1mo
t- 1 to 6mo
t= 1 to 6mo
t < 1mo
4.8
10.5
934
15.0
57.5
4.0
103.0
920
8.9
68.5
7.6
79.1
906
6.8
57.4
3.6
5.7
892
59.6
80.3
7.2
198.0
878
6.1
51.3
864
4.2
105.0
7.0
82.6
5.3
850
123.0
3.7
54.5
6.2
110.0
836
10.6
51.0
T (0C)
985
971
957
943
929
915
901
887
22
-~
Nonannealed
P= 19.6 N
20
CY
0-
ocli
10k
18_
0
Porcelain C
Porcelain V
16k
C
CL
-i
0. 14
cr
0
12 _
0.a.
nI
LI'
I4
1-At&
1.w01
I I I~~~~~~~~~~~~
2
Al
nL+20
-60
-80
-40
AT (0C)
Fig. 9-Pore volume as a function of difference between the actual
firing temperature and the recommended firing temperature.
-20
J'6 V
~~~~~~~~~~~~~~~~~~~~~~~~~~It
Fig
0
SF~~~tim
geolpo
kir r on
por hr V ~ ~ ~
mn
w~~~ld
w
unde
fir d by 56 C
~~~~sistance
TABLE.
5
1.00
Porclain C
Porcelaiii V
1.0
1081
m,
1.12
1.10
' MO
3 mo
1.14
1.18
1. 3
1.22
m
4MO
1.,23
1.321
MO
1.25
37~
ctala
6 fnO
RELFLRVNCLS
12
R(
ACriti
es.
1,39
NIU
ANBKrMRHlF0B11
iue fo
isICin
Mc asremn
Meauinrg~ciur
33
OS
-\~iiS,
nd
ANUSAVIC ii K J RINGt E RD
Values snirirg a Commo ndeln wer rt significantly diffrn.KING Di (1)51 A I in. 51 1oTetfrP rcath Mea Svit Jrs.
i
i69i
Dct Re 6018(
eCOBtE RlKt a KiNGER Y w-!0 196) Litc I Porcwiiwy oi Phyica
specimens showed the largest crack growth in water during the
Si
AIm
J
first month; porcelain V speciiiimens exhibited greater craek
DEHOLv'I.PH. ANUSAVicr K.~an ciS
1. 1983) Anilysis of
BOYCE K9373
growth from the second through the shixt months. We can also
see this effect in the plot Of Pc/2~vM. time in Fig 8. the
paaeter,
is proportional to the s~tressrintenisity factor.
Snethe initial crack sizes were, not significantly different
(p0.05), values ot c/ caar given in TAbl 5 to illustratth
relative growth rates. The horizontal bars indicate values which
aentsignificantly, different (p >.05). The stress orso
susceptibility coefficients wereii consistent with the crack growth
behavior for these specimen. As shown in Tabl 4,n values
were 68.5 and 103.0 for porcelains C an V
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