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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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Effect of Firing Temperature and Water Exposure


on Crack Propagation in Unglazed Porcelain
K.J. ANUSAVICE and R.B. LEE
Departm-nent

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.

.1 Dent Res 68(6):1075-1081, June, 1989

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.

when subjected to transient incompatibility stress below the


threshold stress that produces failure in the presence of spherical voids. Such irregular voids may develop when porcelain
is underfired.
The interactive effects of porosity, residual stress, and water
exposure on crack propagation in dental feldspathic porcelains
have not been previously investigated. Of primary concern is
the effect of residual tensile stress in porcelain veneers of metalceramic restorations caused by thermal contraction mismatch
on crack initiation and propagation. Low-fusing porcelains for
metal-ceramic restorations lack energy-dissipative microstructural features that could significantly enhance the toughness of
these materials. The glass matrix usually contains crystalline
leucite which has the potential to inhibit crack initiation and
propagation. However, Morena et al. (1984) reported a higher
fracture toughness value (1.27 MPa-m"'2) for a high-expansion
experimental frit than for a commercial porcelain (0.88
MPa-m"2). The increased toughness of the experimental materials was attributed to the obstruction of cracks by leucite
particles. The cracks were induced by a Vickers microhardness
indenter which was used for determination of fracture toughness.

Measurements of fracture toughness may provide insight


into analyses of thermal shock resistance of dental porcelain.
In a previous study, Anusavice et al. (1981) measured the
mean thermal shock resistance (reported as AT, the difference
between the annealing temperature and the quenching temperature at which cracking occurred) of metal-opaque porcelainbody porcelain crowns. For one porcelain (Vita body porcelain, shade 540, Vident Corporation, Baldwin Park, CA) with
four types of alloys (Ni-Cr, Au-Pd, Au-Pd-Ag, and Pd-Ag),
the AT value (1700C) was much greater than that (1450C) of
similar crowns fabricated with another commercial porcelain
(Ceramco gingival porcelain, shade Al, Ceramco, Inc., East
Windsor, NJ), even though the transient tensile stress reported
by DeHoff et al. (1983) at the surface of body porcelain in
each case was comparable. Thus, it is possible that this difference could be explained on the basis of potentially greater
fracture toughness of Vita (V) body porcelain.
Recent investigations of the fracture behavior of brittle ceramics have focused mainly on the use of techniques employing controlled surface flaws. These techniques-which include
double torsion, double cantilever, and notched designs (Freiman, 1980)-are not well-suited for materials that are available
in small quantities. For relative fracture toughness comparisons
of dental ceramics, the indentation method is useful (Marshall,
1983; Morena et al., 1984). Another potential benefit of this
method is the ability to produce residual stresses (within the
controlled surface flaw area) which can serve as the driving
force for crack propagation in environmentally sensitive cea

ramics.

The objectives of this study were to investigate the crack


propagation resistance of two body porcelains as a function of
incomplete sintering, and to characterize their susceptibility to
static fatigue by means of the indentation technique. The hypotheses tested were that incomplete sintering enhances crack
1075

1076

J Dent Res June 1989

ANUSA VICE & LEE

-.*- a

No

c0

Fig. 1-Schematic illustration of indentation crack pattern. The initial


crack size (c0) was determined immediately after removal of the microhardness indenter.

growth, and that the higher thermal shock resistance of Vita


body porcelain is a result of its greater fracture toughness.

Materials and methods.


Two commercial body porcelain products, designated as C
and V, were selected for study because of their known thermal
shock behavior. We prepared three bars of each porcelain, 25
mm x 5.5 mm x 5.5 mm, for each set of experimental
conditions. To minimize the effect of residual surface stress
resulting from the formation of a glaze layer and from rapid
cooling, we polished each bar through 0.05 pLm alumina to the
dimensions of 25 mm x 4 mm x 4 mm. We prepared 24
specimens of each porcelain by firing three specimens each (of
porcelain C and porcelain V) in vacuum at 971'C and 920'C,
respectively, and three specimens each in vacuum at a temperature 14'C above, and at temperatures 14AC, 280C, 420C,
560C, 70'C, and 840C below these recommended temperatures. After we polished each bar through 0.05 awm alumina
abrasive, we indented them at six widely separated locations

(3 mm apart) with a load of 19.6 N in a microhardness tester


(Tukon Microhardness Tester, Model MO, Page Wilson Corporation, Bridgeport, CT). Thus, 18 measurements were made
for each condition:
Typical crack patterns, which are shown in Fig. 1, were
produced by the indentation process. We measured the initial
crack length (c0) within two minutes after indentation to minimize errors associated with moisture-enhanced crack growth.
We stored these specimens in distilled water at 370C. We made
subsequent measurements of crack growth at intervals of one
month over a period of six months.
We prepared another series of 48 specimens for each porcelain by firing six specimens at each of the eight temperatures.
We polished the specimens through 0.05 pm alumina, annealed them for 100 h (3520C for porcelain V and 3860C for
porcelain C), and indented them with a load of 19.6 N. We
indented one group of 24 specimens in air and stored it in
water at 370C. We indented another group with a drop of
paraffin oil (to minimize moisture-enhanced crack growth) and
then stored it at 370C in oil. We prepared an additional 15
specimens for each porcelain by firing at the recommended
maturing temperature. We annealed the bars to reduce surface
stresses caused by rapid cooling or grinding. The annealing
temperatures were two-thirds of the glass transition temperature values reported for these porcelains. We avoided higher
annealing temperatures to minimize the risk of microstructural
changes associated with the leucite crystalline phase.
To determine the range of indentation loads in which fracture toughness equations are valid, we indented a group of
three specimens for each porcelain fired at the recommended
temperature at 18 locations with loads (P) of 3.9 N, 7.9 N,
11.8 N, 15.7 N. and 19.6 N. For fracture toughness relations
to be valid, values of P/c 3/2 should be invariant with load
(Marshall, 1983). As for all other specimens, indenter loads
were maintained for 18 sec prior to removal. These specimens
were also stored in test tubes containing water at 370C.
As a reference standard, we used soda-lime-silica glass plates
(microscope slides) measuring 12 mm x 12 mm x 0.9 mm
thick. We embedded the specimens in metallographic mounting resin after annealing them at 3860C for 100 h. We made
30 indentations in each of three specimens at a load of 19.6
N. In one specimen, we made the indentations with a drop of
paraffin oil to minimize slow crack growth resulting from contact of the cracks with atmospheric moisture.
We made all measurements of crack lengths using the microscope of the hardness testing machine. We verified crack
size measurements on specimens with stabilized cracks by means
of a measuring microscope (Unitron, Model BTMD, Unitron
Instruments, Inc., Plainview, NY).
We calculated fracture toughness (K1c) using the relations
developed by Lawn and Fuller (1975) for the residual stress
intensity factor,
Kr = XrP/c3/2
(1)
where c is the crack length, and Xr is defined (Lawn et al.,
1980) by
(2)
Xr - (E/H)
for radial cracks produced by Vickers indentations. If one assumes that the crack system is in equilibrium during and after
the indentation procedure, radial cracks remain stable (c = c,,
and K, = K1c). The applied load (P), modulus of elasticity
(E), hardness (H), and initial crack size (c0) are required for
the calculation of Kc. The calibration constant () for Vickers
indentations is generally taken as 0.016 [according to the calculations of Anstis et al. (1981)] for a variety of reference

1077

CRACK PROPAGATION IN PORCELAIN

Vol. 68 No. 6

ceramics. We calculated hardness values for each indentation


site using the expression,

H = 0.47P/a2

(3)

For soda-lime-silica glass and all porcelain specimens, we


used a value of 73.4 GPa (Wiederhorn, 1969) for the elastic
modulus (E). Although porosity is known to reduce the elastic
modulus of these porcelains, no correction was made, since
data on the variation of E with porosity were not available.
We determined the volume fraction of porosity in each specimen on the indented surfaces by means of quantitative microscopy. We superimposed a 10 x 10 grid on magnified
images of the porcelain surfaces, and performed point-counting
to determine the volume fraction of porosity (Vv), in accordance with procedures described by Underwood (1973). We
divided the number of grid intersection points lying within
pores by the total number of points lying in the grid section
that was superimposed on each microstructure. We made 15
measurements for each group of three specimens.

coefficient (n). The velocity of slow crack growth is usually


described by
dc
K /\n
v
dt V 1K1
(4)
=

where vo is the critical velocity of crack growth at failure, K,


is the stress-intenstty factor, and KIc is the fracture toughness
measured from the indentation method. After indentation, K,
is equal to the right side of Eq. (1). For v,,t/c0 > > 1, Gupta
and Jubb showed that
In

2n
I( 3n+2

In

c =

(322) In t + I

(3n+)

In[(

in[3n+2

(5)
2

VoXr
Kr(,

(6)

where I is the intercept on the In c axis. It follows from Eq.


(5) that the slope of the log c vs. log t plot is equal to 2/

(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

INITIAL CRACK SIZE AND CALCULATED Kic VALUES FOR THE


SODA-LIME-SILICA GLASS REFERENCE STANDARD
CV (%)
c, (>Lm)
Kc (MPa m) CV (%)
7.8
0.73 + 0.03:
10.5
As-received 130.7 4 4.0*
(indented in air)
0.71 + 0.03
10.5
10.4
As-received 132.2 - 5.1
(indented in oil)
19.0
11.9
0.74 + 0.05
130.1 + 5.7
Polished
(indented in air)
*Values preceded by + correspond to the 95% confidence interval for
the mean.

Shown in Fig. 3 is a plot of log c vs. log t for annealed


soda-lime-silica glass specimens indented in air or in paraffin
oil and aged in distilled water and oil, respectively, at 37TC
for three months. [The data points obtained at t = 2 min are
not shown because of the extended time scale.] However, the
mean values fit their respective linear plots very well. "Goodness of fit" values were greater than 97%. Values of stress
corrosion susceptibility coefficient (n) are given in Table 2 for
both as-received and polished specimens at the initial onemonth period and for the period between one and three months.
Values of n were determined from linear regression analyses.
Higher values of n indicate a lower stress corrosion susceptibility.
The value of n found for soda-lime-silica glass specimens
aged in water during the first month (26.5) was higher than
that (14.8) reported by Gupta and Jubb (1981) for the same
indentation load. These authors reported that values of n ranged
between 14.7 and 19.2 for specimens aged in water and between 21.8 and 24.8 for specimens aged in air at room temperature. Gupta and Jubb obtained these data at indentation
0uu

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

J Dent Res June 1989

ANUSA VICE & LEE

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

Annealed Soda-Lime-Slica Glass


2.1
6.(.l1

II

II

6.2

II

6.4

AI

6.6

aI

6.8

7.0

7.2

LOG TIME (sec)


Fig. 3-Log c vs. log t for annealed soda-lime-silica glass specimens
stored in distilled water and oil at 370C.

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

STRESS CORROSION SUSCEPTIBILITY COEFFICIENT (n) FOR


ANNEALED SODA-LIME-SILICA GLASS AGED IN OIL AND
WATER AT 370C
Polished
As-received
Time (mo)
Oil
Water
Oil
Water
0 to 1
105.9
25.2
42.2
26.5
ito 3
20.1
15.7
31.5
20.7

Fig. 4-Effect of firing temperature on fracture toughness of


annealed porcelain C and porcelain V specimens.

slightly greater and is less sensitive to

non-

reduction in firing

temperature.

For the nonannealed specimens in Fig. 4, analysis of Kc


values by the Tukey multiple range test revealed no significant
differences (p>0.05) between the values of specimens underfired by 14'C. For porcelain C, K1c was significantly greater
than that of porcelain V at increments 14AC above (p<0.001),
and 420C (p<0.0002) and 70'C (p<0.04) below their recommended firing temperatures. For the specimens annealed
100 h subsequent to firing, the Tukey multiple range test analysis revealed that the fracture toughness of porcelain C was
significantly greater than that of porcelain V at the recommended firing temperature (p<0.001), and also when underfired by 14AC (p<0.0001), 420C (p<0.0004), 700C (p<0.0001),
and 840C (p<0.03).
Fig. 5 shows initial crack size (co) values (produced by an
indenter load of 19.6 N) for nonannealed specimens as a function of firing temperature. The mean values of co ranged from
87.1 Am (9290C) to 98.5 ,um (971'C) for porcelain C and
from 87.6 ,um (8920C) to 104.0 Aim (934TC) for porcelain V.
Corresponding mean values for annealed specimens ranged from
92.1 rm (9010C) to 106.8 Vtm (915'C) for porcelain C and
99.5 ptm (836TC) to 120.6 VAm (920TC) for porcelain V.
Values of crack size (c) for nonannealed porcelain specimens are plotted in Fig. 6 as a function of firing temperature
and time of exposure in distilled water at 370C. In this case,
the anomalous values corresponding to the firing temperature
of 8920C (see Fig. 5) were excluded for clarity, and to illustrate
the comparative crack growth with increased time. Compared
with the previous Fig. for initial crack length, this plot of crack
lengths for different exposure times resulted in a slightly steeper

CRACK PROPA GA TION IN PORCELAIN

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)

Fig. 7-Log c vs. log t for nonannealed porcelain specimens aged in


distilled water at 370C.

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

indented, and aged in water at 370C for periods of one to six


months. The parameter (P/c3/2) is proportional to K, as defined
in Eq. 1. For the specimens shown in Fig. 8, the residual stress
for crack growth in water has been reduced to an equilibrium
state for porcelain C, while for porcelain V, crack growth is
nearly complete.
The pore volume for each porcelain as a function of the
temperature difference between the actual and recommended
firing temperatures is shown in Fig. 9 for body porcelains C
and V. As shown in this Fig., porcelain C was more sensitive
to void formation when underfired by 40'C or more below the
recommended firing temperature. Pore volumes ranged from
1.6 + 0.2% to 9.4 + 0.7% for porcelain C and from 1.6 -+
0.2% to 5.7 + 0.9% for porcelain V between the recommended firing temperature and a firing temperature 840C below
that recommended.

800

Fig. 6-Crack size of porcelain V specimens as a function of firing


temperature and time of exposure to water at 37TC.

slope and a narrowing of the 95% confidence interval. For


porcelain V, crack growth was progressively suppressed as the
firing temperature was reduced. This relative suppression was
not observed for porcelain C.
Shown in Fig. 7 is a plot of log c as a function of log t for
properly fired (A\T = 0C), nonannealed specimens of porcelains C and V stored in water at 370C. Although the stress
corrosion susceptibility coefficient is higher for porcelain C in
this case, we found no consistent difference between the two
porcelains for either the annealed specimens (Table 3) or nonannealed specimens (Table 4). A 19.6 N indentation load was
used for each case.
Shown in Fig. 8 is a plot of P/C3/2 vs. time for nonannealed
specimens which were fired at the recommended temperatures,

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

J Dent Res June 1989

ANUSA VICE & LEE

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

TIME AFTER INDENTATION (mo)


Fig. 8-Plot of P/C3/2 vs. time determined from nonlinear regression
analysis.

I I I~~~~~~~~~~~~

2
Al

not arrest crack growth in incisal porcelain (C) specimens. The


deflection of cracks away from these particles was attributed
to a radial tensile stress field around each particle.
In our study, we observed cracks passing through both the
centers of pores and along the perimeters of other pores (Fig.
10). Nadeau and Bennett (1978) observed that cracks were
attracted to cylindrical holes (0.5 mm in diameter) with an area
fraction of 0.2 because of the concentrated stress on the diametral plane that is coplanar with the crack. They also concluded that pores can arrest cracks by attracting the crack and
lowering the localized stress. Furthermore, extra energy is expended when the crack curves away from the main crack plane.

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

These mechanisms could explain the crack growth suppression


in porcelain V specimens (Fig. 6) with high void volumes.
For the recommended firing cycle, nonannealed porcelain C

J'6 V

(RCX4K FRUPZ&IalON JA IPORCE1LAIN

for slurries of groundI glass Ileached in water, where AHis the


rectom ntalp). in thi sudy, the inerasd scptibilitf
dental nore lains with aging time nay be icusd hy an in_
er ea I hydroxyl ion concentration at the ira k tip.
is app Aent from Fables 3 and 4 that paraffin oil did not
ad quately pr )tet the crack tips against exposure to trace
qunii s f W tr. This finding
uprtedbyt bcr
fti3n 31u0p't a id Jnbb (198. Othr x igto hase had
little success in eliminating th nluneo moistr re when
I
using tofu ne, mineralI oil, immersion oil, or keros ene Th
post-inldentation growth Of era ks in oil indic ites a high susceptibility of denta porcelains to mhoi'ture-ass e cra' rwh
Becauseo thi senstivity to moistur, means urementso
should be made in dry nittrogen or immediately after ~indentae
of Ki to be obt mned.
ton in order for acr svli
The absence of a clear trenidtoward stres corrosion suscep-~
tibility when firn ~ te uperature is decersed snggets th t porosity h is little effect on moilture-asited crack growth, Possibly
because the pores an ctious and becarl tecon, Am
r that Cannot rdiybe displaced by water near the rk
ic
enhanced thirmal
suggV st that the likelyba
tip. lbeseresnts
islt of shock
of 'p
its~lower
may more
~~~~~~~~~~~~~snseeptibility to s ress corrosion at the initial stage of crack
propagation.

~~~~~~~~~~~~~~~~~~~~~~~~~~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

RELA lVE CRACK GROWTH IN WATER AT 37 C


min

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

vrrrtrr o iiniiafio Tec

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

i~

Sr

i kIrM1S

iI)lt6 9

R MNSW 1811i
echiiniigy, DRK uhimin
iiI'K ttnuN

M
d

NJ

sI(ts cec n

K id ss, N' wYork Academic


iSwCxs
Pi

C~6si

JONE S

14
6~ss Ai CemS10 64-C '1
tini
W TONiES P.A. in WItLSON, 11L1 117) Iiei:
thii iid T1 i M ii~abieta)i rm

N5

SNi

Sit

Ii

13iiCii

rspctveyin!
Ra in 203t6.
LANnviv\Sx

fist Month, while the values decicrased to 8,.9 arid 4.0,


~therespectively,
in the second through sixth months.

aMA.Ixi (I 9811 ii i p1sle


I
rDr.iCriiI iiiK11iinSy i i/An
Ci S
The values of n determined in the first month fore the an
.
LAWN FBIR FriFLP I
F17)Eqifir Fe -ikvS
sealed speiens (fable 3) are, similar to te valued of 39 o
Fra jr Alaier
e
i
atamied by Somna et al. (1980)~for porcelain consisting of a glass
c
MARSHALLFDu i1
otrl~ flaws
rrsip
and crstalline particlesof mulie qatz, and corunm
Knp n Vi e ii taioiii/ CcrSo i6612
M Ik 1(/K1,)P
A L~
~Ri
dum. This susceptibility to stress corrosion could be3 a result
C T1 aI Po(4tlu
uhsicC
Mr~il
ri
Of thieincrease in hydroxyl, ion Concentration at the tip of the
6 234 Ah
I JDeno R~
1 5 Mertsu t Dise isedl Piae
radial crack frontts. Wiederhorin (1972) hy~pothesized that hyNADEAI
J.S HnENNLETT, KC. (I97)
r
ii
vior
ii,s
Frctr MhaIc (PCramnics,
droxyltons attack- siloxane bonds Rand that silanolate group
ilnl rup4ndh Pr 'cig
atriernai Syr
M~anccl
chan be hydrolyzed by waeWtIor
C
l
IH
'ai
t
c
woinu
droxyl ions throughh the reaction:
Prss n0 961-97
AEILLi C P BL W (In3536
oH
K
iU
i R
K ISiuH
R SiDt
7)TI verse Si gn t ItniiAuu
(7)

~matrix

SiO

H20 ~R

SiOH

OH

()

He supported this hypothesis with data which showN~ed anL increase


Iin crack velocity, with increasing hydr~oxyl ion concentration.
T1he aging temperatures should also affect the stress corsio

Vad
Foce tiir!JcR'
~
6)3~0
151i YMM~ENi8Apiiiti
soM T.Fredpti
MAITSUL
Cr(3 F 69 iDoiLirPIi
iPr1r ACa
5 0:66-i
iph In.
E-Et 173).A I c 'rii1 Oalliv54rit
Metals Hiandbouk, V61 Meto ~y Sfr ie cld P i Diiia Kng

UNtDiRWOO0

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