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.

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.

.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.

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

ANUSA VICE & LEE

J Dent Res June 1989

-.*- 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

Vol. 68 No. 6

CRACK PROPAGATION IN PORCELAIN

1077

ceramics. We calculated hardness values for each indentation site using the expression,

H = 0.47P/a2

(3)

coefficient (n). The velocity of slow crack growth is usually described by dc K v dt V 1K1 /\n (4)
=

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.

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
c =

(322) In t + I

(5)
2
VoXr
Kr(,

2n I( 3n+2

In

(3n+)

in[3n+2

In[(

(6)

where I is the intercepton the In c axis. It follows from Eq. (5) that the slope of the log c vs. log t plot is equal to 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 ofK1c (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

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

(3n + 2).

Porcelain C
cam

E
Cu

acm

I0
100

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.

to0

0~
Porcelain V

20 15 10 LOAD (N) Fig. 2-Load-crack size parameter, P/c,, as a function of load.

1 I 0,

25

1078

ANUSA VICE & LEE

J Dent Res June 1989

TIME (sec)

2.3 F

:6
I
I I
I I

I 07
1 I1 1

.6

P=19.6 N
E
w

.4

1.2

water

n2=0.7
.0
CLJ

en U

Cll

2.2

oil

n=31.5

0.8

cm

0b
0

CD
0

Annealed Soda-Lime-Slica Glass

2.1 6.(.l1
I I

II

II

AI

I a

6.2

6.4

6.6

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
non-

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

Fig. 4-Effect of firing temperature on fracture toughness of annealed porcelain C and porcelain V specimens.

slightly greater and is less sensitive to

temperature.

reduction in firing

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

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

Vol. 68 No. 6
1 10

CRACK PROPA GA TION IN PORCELAIN

-10 lbalr

1079

100
E
0

Porcelain C P=19.6 N

150

Nonannealed P=19.6 N

901
01
I
I

a n - - _~ ~ ~ ~ ~ - t
, -' s , , ,~~~~~~~~ ,- , ~ ,I I I I

140 F
_

co

ii N

:x

130_
120_
n=8.9

11U.

980

960

940

920

900

81 30

L N

C.)
-J

Vo
Porcelain V
C.
---..

I1100

cc

OF

o0II

LI

940

920

900

880

860

840

T (0C) Fig. 5-Initial crack size, c,, vs. firing temperature for nonannealed

90 ,

I l I I I I

106

107
TIME AFTER INDENTATION (sec)

porcelain specimens.
7;;
.

Fig. 7-Log c vs. log t for nonannealed porcelain specimens aged in distilled water at 370C.

120

~~~Porcelain V ~~~ <

I,110
LL
~~~~~~~~~,

la P

~~ ~ ~ ~ 1 ~ mosI

C)

--I~~~~~~~~~~~~~t 2 min
00o
li

90h

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.

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

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,

1080

ANUSA VICE & LEE

J Dent Res June 1989

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
I

T (0C)

985 971
957 943 929 915 901 887
22

-~

ocli

20
CY

Nonannealed P= 19.6 N

10k

18_
0

E
0-

Porcelain C Porcelain V

16k
C
-i

CL

0. 14
12 _
nI LI'

cr 0

a. 0.
I4
I
I

A 1- t&

6
I I I~~~~~~~~~~~~

TIME AFTER INDENTATION (mo) Fig. 8-Plot of P/C3/2 vs. time determined from nonlinear regression analysis.

1.w01
2
Al

not arrest crack growth in incisal porcelain (C) specimens. The deflection of cracks away from these particles was attributed to aradial 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.

-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

nL+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& alON JA IPORCE1LAIN I

1081

mn fir d by 56 C w~~~ld w unde ~~~~sistance TABLE. 5

Fig 0 SF~~~tim r on geolpo kir

por hr V ~ ~ ~

RELA lVE CRACK GROWTH IN WATER AT 37 C

min

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 ton in order for acr svli of Ki to be obt mned. 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 tip. lbeseresnts sugg may the likelyba thirmal shock ic st that enhanced islt of its~lower V of 'p more ~~~~~~~~~~~~~snseeptibility to s ress corrosion at the initial stage of crack propagation.

~~~~~~~~~~~~~~~~~~~~~~~~~~It

ctala

Porclain C

1.00

m, 1.12

' MO

3 mo

1.14

1.18

m 4MO 1.,23

MO

6 fnO
12 N S R( NIU

RELFLRVNCLS
ANBKrMRHlF0B11
iue fo

1.25

Porcelaiii V

1.0

1.10

1. 3

1.22

1.321

37~

1,39

ACriti

es.

vrrrtrr o iiniiafio Tec

isICin Mc asremn

Meauinrg~ciur

33

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 ar (p0.05), values ot c/ ca 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
while the values ~the fist Month, the second through decicrased to 8,.9 arid 4.0, sixth months. respectively, in
were 68.5 and 103.0 for porcelains C an V

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 1o frP rcath Mea Svit Jrs. Tet i Dct Re 6018( i69i eCOBtE RlK a KiNGER Y w-!- 196) Litc I Porcwiiwy oi Phyica t 0 specimens showed the largest crack growth in water during the AIm J an BOYCE 9373 first month; porcelain V speciiiimens exhibited greater craek DEHOLv'I.PH. Si ANUSAVicr K.~ ciS K 1. 1983) Anilysis of

i~

Sr

i kIrM1S M
d

iI)lt6 9

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

NJ

K id ss, N' wYork Academic iSwCxs Pi

sI(ts cec n

JONE S

C~6si

14 S 6~ss Ai Cem 10 64-C '1 tini W TONiES P.A. in WItLSON, 11L1 117) Iiei: thii iid T1 i M ii~ biea) rm a ti

N5

SNi

Sit

Ii

13iiCii

~matrix

i aMA.Ix (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 S LAWN FBIR FriFLP I F17)Eqifir Fe -ikv . sealed speiens (fable 3) are, similar to te valued of 39 o Fra jr Alaier e otrl~ flaws ic atamied by Somna et al. (1980)~for porcelain consisting of a glass MARSHALL Du i1 F 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 I JDeno uhsicC (4tlu R~ 234 Ah Mr~il ri Of thieincrease in hydroxyl, ion Concentration at the tip of the 6 1 5 radial crack frontts. Wiederhorin (1972) hy~pothesized that hyNADEAI J.S HnENNLETT, KC.,s (I97)Frctr Mertsu t Dise isedl Piae r ii vior ii MhaIc (PCramnics, droxyltons attack- siloxane bonds Rand that silanolate group ilnl rup4ndh atriernai Syr M~anccl chan be hydrolyzed by waeWtIor Pr 'cig C l IH 'ai t c woinu droxyl ions throughh the reaction: Prss n0 961-97 AEILLi C P BL W (In7) verse Si gn t ItniiAuu oH K iU i R K ISiuH R SiDt 3 TI (7) 536
V

rspctveyin! Ra in 203t6. LANnviv\Sx

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

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

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