J. Am. Ceram. Soc.
, 85 [7] 1777– 82 (2002)
journal
Biaxial Flexure Strength and Dynamic Fatigue of
Soda–Lime–Silica Float Glass
Matthew H. Krohn, John R. Hellmann,* David L. Shelleman,* and Carlo G. Pantano*
Department of Materials Science and Engineering, Materials Research Institute, The Pennsylvania State University,
The strength and dynamic fatigue behavior of float glass was
investigated using biaxial flexure tests. The samples were
tested using the ring-on-ring (ROR) biaxial flexure test geom-
etry, and the data analyzed using a conventional two-
parameter Weibull distribution. The as-received samples re-
vealed that the air side exhibits a higher characteristic strength
(243 MPa) compared with the tin side (114 MPa); fracto-
graphic analysis confirmed the presence of significantly larger
flaws on the tin side of the specimens, presumably due to
contact damage by the rollers in the float glass process.
Dynamic fatigue results for as-received and indented samples
were performed to assess whether differences in the stress
corrosion behavior of float glass exist because of tin penetra-
tion. No statistical difference in the stress corrosion exponent
was found between the air (n ⴝ 21.7) and tin (n ⴝ 21.6) sides
of the float glass. This indicates either that the tin penetration
(which extends ⬃25 ␮m) plays no role in altering the stress
corrosion susceptibility of float glasses because the native flaw
size is larger than the tin penetration depth or that the tests do
not have the required sensitivity to distinguish the effect of the
tin. Alternative test methods for direct observation of slow
crack growth in tin-doped bulk glasses are planned to inves-
tigate this in the future.
I. Introduction
I N THE early 1960s, Pilkington Brothers Ltd. introduced the float
process for the production of flat glass.1 The float process offers
continuous mass production of flat glass with an excellent surface
finish with no secondary processing steps required. The float
process is the principal method for the production of flat glass
throughout the world. Float glass is used in a variety of applica-
tions, including automotive and architectural enclosures.
Glass produced using the float process contains a significant
amount of tin diffused into the surface in contact with the molten
tin bath (tin side.) The surface of the glass exposed to the
atmosphere (air side) contains a negligible amount of tin compared
with the tin side. The diffusion profile of the tin into the glass is
related to numerous variables such as glass composition, glass
redox, ion exchange between the glass and constituents in the tin
bath, oxygen and metallic contamination of the tin bath, float bath
K. T. Faber—contributing editor
Manuscript No. 187391. Received October 22, 2001; approved April 26, 2002.
This work is funded by the NSF Industry–University Center for Glass Research,
Site for Glass Surfaces and Interfaces Research, at the Pennsylvania State University,
Project No. EEC-9908423.
*Member, American Ceramic Society.
1777
University Park, Pennsylvania 16802
George E. Sakoske*
Ferro Corporation, Washington, Pennsylvania 15301
atmosphere, temperature, and time on the float bath.2 The chem-
istry of the tin side of the float glass has been the focus of many
studies.3–14 It is generally accepted that the tin penetration on the
tin side ranges from 10 to 40 ␮m, and is present in both the
stannous (Sn2⫹) and stannic (Sn4⫹) forms. The stannous form is
more prevalent near the surface, while in the subsurface tail of the
diffusion profile the stannic form predominates. Furthermore, the
diffusion profiles obtained in most studies exhibit a characteristic
“bump” in the subsurface region, approximately halfway through
the tin penetration depth3,4 (see Fig. 1). This has been attributed to
the accumulation of the slower diffusing stannic form in the
subsurface where the local oxidation potential is increasing.
The local structure of the stannic and stannous species in the
glass structure remains a subject of significant debate.12,13 It is
generally accepted that the Sn2⫹ is accommodated as an interme-
diate or network-modifying cation,15 but the coordination of Sn4⫹
is less well understood. Although Sn4⫹ exhibits very low solubility
in pure silica, recent NMR studies suggest that small concentra-
tions of Sn4⫹ can be accommodated, at least partially, as a
network-forming cation (i.e., substitute for Sn4⫹).16 This is con-
sistent with the lower diffusion coefficient of Sn4⫹. Other studies,
using Mössbauer spectroscopy, suggest that Sn4⫹ is accommo-
dated in a significantly more covalently bonded, rigid arrangement
than the Sn2⫹.12 This may lead to speculation that scission of
network bonds may occur differently in tin-doped silicate glasses,
leading to differences in slow crack growth behavior.
The effect of tin concentration and oxidation state on the
physical properties of SnO–SiO2 glasses has been well-studied.17
In addition, there is substantial evidence that shows the tin side of
thermally toughened float glass exhibits enhanced resistance to
contact damage compared with the air side.18 However, the role of
tin on the strength and slow crack growth behavior of soda–lime–
silica float glass has seen only limited study; the repeated results
and interpretations are not consistent.19,21
In an early study, Tummala and Foster19 reported higher
strengths for the air relative to the tin side of float glass, and a
higher stress corrosion resistance of both sides relative to soda–
lime–silica rods.20 They attributed the higher strength on the air
side to a higher level of compressive stress, which arises from
alkali and alkaline-earth depletion during the float process. Fur-
thermore, they reported a reversal of that effect at high mechanical
stressing rates (i.e., the tin side was stronger than the air side of the
glass,), which they interpreted as being due to a higher resistance
to environmentally enhanced slow crack growth for the tin side of
the float glass. However, on close examination of their data, it is
questionable as to whether there is a statistically significant
difference in the stress corrosion exponent (n) derived from their
dynamic fatigue tests for the air versus tin side of the float glass
specimens.
Later work by Akcakaya et al.21 confirmed that the air side of
float glass is generally stronger than the tin side, presumably
because of the greater flaw severity due to contact damage induced

1778 Journal of the American Ceramic Society—Krohn et al.
Fig. 1. Typical tin penetration profile for PPG Solex float glass.
by the rollers on the tin side of the glass as it exits the float process.
More interestingly, however, is that they also report a difference in
the stress corrosion behavior of the air versus tin side of the float
glass, with the air side being more resistant to stress corrosion.
This is in conflict with Tummala et al.,19 and further confuses the
issue regarding the effect of tin on the fatigue resistance of float
glass.
Therefore, the focus of this investigation was to examine
whether differences in the strength and dynamic fatigue behavior
exists between the chemically different surfaces of float glass.
Biaxial flexure testing, as a function of stressing rate, is combined
with indentation strength studies and fractographic analysis to
interrogate differences in strength and stress corrosion susceptibil-
ity of a commercially available float glass.
II. Experimental Procedure
Commercial soda–lime–silica float glass plates (SolexTM, PPG
Industries, Inc., Pittsburgh, PA) were procured for biaxial flexure
tests. Half of the specimens were tested in the as-received
(well-annealed by manufacturer) state, while the other half were
subjected to a heat treatment aimed at simulating an enamel-
decorating process. The heat treatment consisted of a 10 min firing
at 480°C, a 4 min ramp to 645°C, a soak at 645°C for 6 min,
cooling below 480°C in a 15 min period, and air cooling to
room temperature. The square plate samples measured an
average of 76.3 ⫾ 0.5 mm on an edge and had an average
thickness of 3.89 ⫾ 0.02 mm.
(1) Strength Test Methodology
Ring-on-ring (ROR) biaxial flexure tests were used for strength
tests on the air and tin sides of the glasses, in the as-received and
heat-treated conditions. The biaxial flexure test fixture was de-
signed based on a draft test standard currently under review by the
ASTM Subcommittee C28.01 on Properties and Performance.22
The fixture comprised a support ring of diameter of 52.07 mm and
a concentric loading ring of 22.86 mm diameter. Each ring had a
radius of curvature of 2 mm, and was fabricated from 17-4PH
stainless steel (see Fig. 2).
An Instron (Model 4202, Instron Corp., Canton, MA) load
frame was used to drive the loading ram. GrafoilTM (UCAR
International, Inc., Nashville, TN) sheets (0.381 mm thick) were
used to reduce friction and serve as a compliant layer between the
sample and the support and load rings. For the higher strength
samples (air side) manila paper was added between the rings and
the Grafoil to retain the Grafoil layer. Adhesive tape was applied
to the compressive side of the sample to retain fragments for
fractographic analysis.
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Vol. 85, No. 7
Fig. 2. Cross-section schematic of the fixture used for the ROR biaxial
flexure tests.
Twenty five to fifty specimens were tested for each condition,
at a stressing rate of 2.0 MPa/s, and the loads to failure were used
to calculate the strengths of the specimens using analyses derived
by Roark and Young23 or Timoshenko and Woinowsky-Krieger.24
A term to account for the overhang of the samples, introduced by
Vitman and Pukh,25 was used in the stress calculations. The
equation used to calculate the maximum stress generated in the
ROR tests is
冋 冉 冊 冉 冊册
3P R2L RS2 RS
␴ Max
ROR
⫽ 2 共1 ⫺ ␯兲 1 ⫺ 2 2 ⫹ 2共1 ⫹ ␯兲 ln (1)
4␲h RS R RL
where P is the applied load, h is the thickness, ␯ is Poisson’s ratio,
R is the radius of the samples, which is the average of the edge
length and the body diagonal, RS is the radius of the support ring,
and RL is the radius of the load ring.
The strength distributions were analyzed using a conventional
two-parameter Weibull approach;26 the Weibull parameters were
calculated using maximum likelihood estimators (MLEs) using a
Microsoft Excel Macro developed at Cleveland State University
by Baker and Duffy.27 The MLE fits along with unbiasing factors
were used to determine the unbiased Weibull moduli and charac-
teristic strengths.
(2) Dynamic Fatigue Tests
Heat-treated float glass plates were used for the dynamic fatigue
tests. Half were tested with the air side in tension and the other half
with the tin side in tension. Specimens were initially tested with
the native surface flaw populations similar to other studies that
investigated the dynamic fatigue behavior of float glass;19,21
however, it was found that these tests yielded unacceptable scatter
in the data. To improve the precision of the measurements, and to
permit an unambiguous determination of the stress corrosion
exponent from the dynamic fatigue plots, the experiments were
repeated using specimens in which well-controlled flaws were
introduced via indentation. Indents were introduced on the tensile
side using a Vickers hardness micro-indenter (Model MHT 200,
LECO Corp., St. Joseph, MI) at a load of 300 N for 15 s. To ensure
the complete development of the flaw geometry, the samples were
 15512916, 2002, 7, Downloaded from https://ceramics.onlinelibrary.wiley.com/doi/10.1111/j.1151-2916.2002.tb00352.x by Czech Technical University, Wiley Online Library on [02/06/2023]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
July 2002 Biaxial Flexure Strength and Dynamic Fatigue of Soda–Lime–Silica Float Glass 1779

Fig. 3. Two-parameter Weibull plots for heat-treated and as-received, 76-mm, unenameled Solex samples tested using a ROR biaxial flexure test at a
stressing rate of 2 MPa/s. The unbiased Weibull modulus (m) characteristic strength (␴␪), and the number of specimens tested (N) are displayed in the graph.
The values in the parentheses represent 90% confidence intervals for N specimens.

exposed to the atmosphere for a 24 h period. The indented samples
were fractured at five different stressing rates ranging from 0.020
to 200 MPa/s, using the ROR test geometry. Silicon oil was
applied to five of the indented samples after the 24 h flaw
development period. These samples where then tested to determine
the inert strength of the indented samples.
The loads at fracture were recorded and the stresses were
calculated using Eq. (1), and the stress corrosion exponent (n) was
calculated from the plots of strength versus stressing rate accord-
ing to analyses derived by Charles30 and Evans:31
III. Results
(1) Biaxial Strength Tests
The results from the ROR tests of the as-received and heat-
treated samples are shown in Fig. 3 and Table I. Two important
results are evident. First, there is a significant difference in the
characteristic strength and Weibull modulus between the air- and
tin-side surfaces. The characteristic strength of the tin-side samples
is significantly lower than that of the air-side samples: 125 MPa
compared with 248 MPa for the as-received samples and 114 MPa
compared with 243 MPa for the heat-treated samples. The Weibull

冋 冉 冊册 moduli of the tin-side samples are slightly higher than the air-side
1/共1⫹n兲
d␴
␴f ⫽ ␤ (2) samples: 5.6 compared with 3.8 for the as-received samples and
dt
6.9 compared with 4.0 for the hear-treated samples. Second, heat
treatment does not anneal-out this difference in strength between
where ␴f is the fracture stress, ␤ is a constant, d␴/dt is the stressing the air and tin sides. It does have a small effect on the characteristic
rate, and n is the stress corrosion exponent. The stress corrosion strength of the tin side. The fractography revealed that the critical
exponents calculated from the plots were corrected for the residual flaws present on the tin side’s surface are larger compared with
stresses that resulted from the indents and contact-induced those found on the surfaces of air-side samples (Fig. 4), which
flaws.28,29 explains the lower characteristic strengths of the tin-side samples
shown in Fig. 3. The critical flaw sizes (a) were calculated for the
tested samples using the following equation:
(3) Fractography
Fractographic analysis was conducted on the samples to identify
the types of failure origins that contributed to failure. Visual
inspections of the samples determined the location of the fracture
a⫽ 冉 冊
K IC
␴fY
2
(3)

mirrors and whether the sample had failed from surface or volume
flaws. Special attention was placed on identifying samples that
failed under the load ring or from edge failures. Optical micros-
copy was also helpful in determining the type of failures. Selected
fracture mirrors were investigated using scanning electron micros-
copy (SEM) to define typical fracture origins.
where KIC is the fracture toughness (0.76 MPa䡠m1/2), Y is a
geometric parameter (2.24/␲1/2 for a half penny surface crack),
and ␴f is the stress at failure. The results of the calculations (Table
I) corroborated the findings of the fractographic analysis, confirm-
ing that the average critical flaw found on the tin side is larger than

Table I. Unbiased Weibull Moduli (m), Unbiased Characteristic Strengths (␴␪),

Critical Crack Sizes (a), and Number of Specimens Tested (N) for
As-Received and Heat-Treated Samples†
As-received Heat-treated
Tin Air Tin Air

m 5.6 (4.7, 6.9) 3.8 (3.1, 4.4) 6.9 (5.4, 8.8) 4.0 (3.1, 5.1)
␴␪ (MPa) 125 (120, 131) 248 (232, 265) 114 (109, 119) 243 (224, 265)
a (␮m) 28.9 ⫾ 9.7 13.0 ⫾ 17.3 35.6 ⫾ 17.9 10.2 ⫾ 8.3
N 55 51 29 28
†
Numbers in parentheses represent 90% confidence intervals on N specimens.
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1780 Journal of the American Ceramic Society—Krohn et al. Vol. 85, No. 7

Fig. 4. Typical flaws found on the chemically different surfaces of float glass: (a.) air-side (left side fracture mirror, right side fracture origin) flaw size ⬇
10.2 ␮m; (b) tin-side (left side fracture mirror, right side fracture origin) flaw size ⬇ 35.6 ␮m.

the average critical flaw found on the air side for both the
as-received and heat-treated samples.
There is some evidence for a second flaw population to be
contributing to the low strength of the float glass specimens.
Fractography reveals that flaw type appears the same, but they are
merely larger. It is possible that handling introduced these larger
flaws, but censoring the data to incorporate two different flaw
types is not warranted as there is no apparent difference in type,
other than size, in this case.
(2) Dynamic Fatigue
Preliminary measurements, performed using a ball-on-ring test
geometry on a limited number of specimens, did not reveal a
statistically significant difference in the stress corrosion exponent
for the tin-side versus air-side specimens (Fig. 5.) However, the
precision of the strength data as a function of stressing rate yielded
unacceptably large bounds on the value of the stress corrosion
exponent. Therefore, the experiments were repeated using the
ROR geometry, with a larger number of specimens, into which
well-defined flaws had been introduced using a Vickers indenter.

Fig. 5. Dynamic fatigue plot for 105 mm Solex samples containing native
flaws tested using the BOR test geometry. n values have been corrected for Fig. 6. Dynamic fatigue plot for 76 mm unenameled indented Solex float
the residual stress, which results from the contact-induced native flaws glass; n values have been corrected for the residual stress, which result
(parentheses denote the 95% confidence intervals). from the indentation (parentheses denote the 95% confidence intervals).

July 2002 Biaxial Flexure Strength and Dynamic Fatigue of Soda–Lime–Silica Float Glass
Fig. 7. Schematic of the average depth of the median-radial cracks (33
␮m) produced by the Vickers indents relative to the tin penetration depth,
showing that the cracks extend through the tin penetration region.
The indents produced median-radial cracks with crack lengths of
66.5 ⫾ 2.8 ␮m for the samples indented on the tin side and 62.9 ⫾
2.7 ␮m for the samples indented on the air side. During the 24 h
flaw development period, the median-radial cracks grew an aver-
age of 7.9 ⫾ 3.3 ␮m on the tin side and 5.9 ⫾ 2.9 ␮m on the air
side. The results from the strength tests on indented specimens are
shown in Fig. 6.
These results corroborate those of the unindented specimens,
and illustrate that no difference in the n values is detected for the
air side (21.7(20.4,23.2)) and tin side (21.6(19.6,23.9)) of the float
glass. These values are in good agreement with typical values
reported for soda–lime–silica glass (n ⫽ 16 to 22).20,28 –33
It has been shown in the literature that the tin-rich zone in the
float glass has different properties relative to the bulk glass and the
air side.10,17,34 –37 It would be expected that this difference in
properties would lead to a difference in the stress corrosion
susceptibility of the two surfaces of the float glass. That this
difference was not observed in this study is possibly due to the
depth of the cracks introduced by the indents being comparable to,
or larger than, the tin penetration depth (Fig. 7). Therefore, only a
small fraction of the crack tip will reside in the tin penetration zone
during crack extension. This may mask the effect that tin has on
the stress corrosion susceptibility of the float glass, as measured by
dynamic fatigue methods. A better method for determining the
effect of tin on the stress corrosion susceptibility of soda–lime–
silica glass may be via direct observation of crack growth as a
function of stress intensity on bulk glasses synthesized with
different tin concentrations. Applied moment double cantilever
beam experiments are planned for the future to interrogate this
hypothesis.
IV. Summary
The objective of this study was to determine the strength and
stress corrosion susceptibility of the two chemically different
surfaces of soda–lime–silica float glass. ROR biaxial flexure tests,
with the air side versus the tin side in tension revealed that the air
side of the glass has a higher characteristic strength and lower
Weibull modulus compared with the tin side. The lower charac-
teristic strength of the tin side of the glass has previously been
attributed to the presence of larger flaws, apparently due to contact
damage induced by the rollers supporting the glass at the end of the
float glass fabrication line.21 The presence of larger flaws on the
tin side of the float glass was confirmed by our fractography. It is
not known whether the tin enhances or limits flaw generation due
to this contact based on the data obtained here. Dynamic fatigue
tests on virgin and indented specimens revealed no difference
between the stress corrosion exponents for the air and tin sides of
the float glass. More sensitive experiments, such as direct obser-
vation of slow crack growth as a function of applied stress, are
15512916, 2002, 7, Downloaded from https://ceramics.onlinelibrary.wiley.com/doi/10.1111/j.1151-2916.2002.tb00352.x by Czech Technical University, Wiley Online Library on [02/06/2023]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
1781
needed to unambiguously interrogate the effect of the tin on the
stress corrosion behavior of float glass.
Acknowledgments
We thank Drs. John Salem and David Green for their stimulating conversations.
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1782 Journal of the American Ceramic Society—Krohn et al. Vol. 85, No. 7
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