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Journal of Non-Crystalline Solids


journal homepage: www.elsevier.com/locate/jnoncrysol

Glasses: New approach to fracture behavior analysis


George A. Gogotsi *, Sergey P. Mudrik
Pisarenko Institute for Problems of Strength, 2, Timiryazevskaya Str., 01014 Kiev, Ukraine

a r t i c l e i n f o a b s t r a c t

Article history: The rectangular specimen edges of optical and technical glasses were fractured in the tests with conical
Received 4 June 2009 indenters and pyramids. It was demonstrated that in the Rockwell indentation, away from those edges a
Received in revised form 11 January 2010 ring crack and a Hertzian cone were formed. But when the indentation point approaches the specimen
Available online xxxx
edge, only fragments of ring cracks develop and chip scars look like a Hertzian quasi-cone. The behavior
of glasses was investigated with the edge fracture (EF) test method. It is shown that the fracture resis-
Keywords: tance of oat glass is higher than that of fused silica and other optical glasses, the lowest fracture resis-
Glasses
tance is displayed by heavy int. When glass surfaces are indented by a Berkovich indenter, lead glasses
Fracture
Indentation
exhibit a better fracture resistance. It was revealed that glasses possessed the barrier to the onset of frac-
Optical microscopy ture, not typical of conventional brittle materials. The results conrm that the time- and cost-saving EF
Microstructure test method can be quite promising for comparative estimates of the ability of glasses to resist fracture.
Oxide glasses 2010 Elsevier B.V. All rights reserved.
Sodalimesilica
Structure
Defects
Chip scar
Edge aking (chipping)

1. Introduction [6] (also conrmed in Ref. [7]) that IF methods are inappropriate
for any basic fracture resistance measurements of ceramics or
Silicate glasses are so much a part of our everyday lives that any other materials. Moreover, evaluation of fracture resistance
they are perceived as something self-evident [1]. These low- of glasses with any indenters is of academic rather than of practical
deformable elastic materials prone to catastrophic fracture can signicance since such local damages do not control a real carrying
be scratched quite easily on their surfaces, and their edges are sen- capacity of this material.
sitive to chipping. Thus, the fracture behavior that often exerts Therefore, a concept of evaluating the fracture resistance of
negative inuence on the performance of these materials has long glasses is coming into use [8]. It consists in aking the rectangular
received much investigation [2]. specimen edge that resembles the tests of stones in ancient times
The ability of glasses to resist fracture is usually characterized to choose them for making arms and tools [9]. It is not based on
by the critical stress intensity factor KIc [3], which, however, is any models and provides direct measurements of the fracture
not aimed at engineering calculations of glass items, it basically resistance of brittle materials. The performance of such a method
fullls the role of a comparative numerical guide for evaluating (version termed the edge fracture (EF) test method [10])1 was dem-
the ability of glasses to resist fracture under mechanical loads. onstrated, e.g., with studies on the fracture behavior of several brittle
For determining this factor, conventional test methods, based on materials [1315]. It was revealed that quartz glass exhibited a high-
the linear fracture mechanics concepts [1,3], are usually used, er barrier to the onset of fracture, which is typical of silicon or boron
which were earlier developed to estimate the properties of metals carbide-based ceramics used for manufacturing armor, but which is
and ceramics. Glasses are also tested by the Hertzian indentation not observed in conventional brittle materials [11].
(ball indenter) and Vickers indentation fracture (IF) methods Quite a number of studies on different ceramics with the EF test
[1,4]. The disadvantage of the conventional methods is the require- method [10] gave rather promising results that suggested an idea
ment for comparatively substantial mate (or appropriate), and to extend this approach to glasses. Thus, investigations aimed at
Hertzian indentation tests are difcultly realizable in a normal the fracture behavior of these materials were performed. Their re-
mechanical laboratory [5]. Analysis of publications demonstrates sults became the subject matter of the present communication.

* Corresponding author. Tel.: +380 44 285 44 64; fax: +380 44 286 16 84.
1
E-mail address: ggogotsi@ipp.kiev.ua (G.A. Gogotsi). Comparison of similar test methods was performed in Refs. [11,12].

0022-3093/$ - see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jnoncrysol.2010.01.021

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Table 1
Characteristics of optical glasses.

Glass Density (g/cm3) Composition (%) Refractive index Adobe Number


SiO2 PbO K2O As2O3 Sb2O3 nc nD Vd

RI fused silica 2.21 99.8 1.4601 1.4584 67.83


TF-2 heavy int 3.86 39.1 55.41 4.94 0.25 0.30 1.6522 1.6475 33.86

Table 2
Experimental results.

Glass Elastic modulus (GPa) Hardness (GPa) KIc (MPa m1/2) Fracture resistance (N/mm)
FR FR400 FRV FRB
a
RI fused silica 73.6 224 66(151) 269 72(51) 101 12(48) 79 15(45)
TF-2 heavy int 56.1 4.57 0.83 192 31(100) 203 60(54) 77 18(50) 127 36(42)
Neodymium glass 6.07 0.84 228 50(64) 106 23(51) 64 18(39)
Float glass 73.4 6.61 1.03 241 55(115) 251 67(52) 124 24(62)
F-2 int 4.71 0.85 192 41(42) 97 21(49) 117 31(32)
a
Number of chip scars.

2. Experimental applied loads. The next step was microscopic analysis of experi-
mental results with a BX51M Olympus binocular microscope
The objective of this investigation was to evaluate the ability of (501000) using a QuickPHOTO MICRO 2.3 program. After visual
glasses to resist the aking of their edges and to study their frac- analysis, indenter imprints and chip scars were photographed in
ture behavior under these conditions. High-quality optical silicate reected light.
glasses, manufactured in accordance with the Standards of the for- The fracture resistance of glasses was evaluated by the ratio of
mer USSR [16,17], normal oat glass, and neodymium glass2, used the load Pf, applied to a Rockwell indenter, to the distance L, mea-
in rst Soviet solid lasers, were chosen as key materials, an F-2 int sured from the specimen edge to the extreme point of the chip scar
glass [17] served as an auxiliary material (Tables 1 and 2). The tests on its surface (Fig. 1). This operation was multiple-repeated, thus,
for certication of glasses included evaluation of hardness [18] and the fracture resistance of the material was characterized by the
fracture toughness [19] by the Vickers indentation. Tests were per- average ratio designated as FR. Studies on glass fracture behavior
formed on 3  4  25 mm3 rectangular bars with an edge radius less were performed under spherical, linear, and point contacts of an
than a micron. They were cut from the middle part of glass stock, indenter with glass surfaces [4], using blunt indenters (Rockwell
which excluded a possible effect of its surfaces on glass properties. and cone) and sharp indenters (Vickers pyramid for microindenta-
To form rectangular edges, the bars with polished sides tion, and Berkovich pyramid with sharpening for nanoindentation).
(4  25 mm2) were rst prepared. Then they were glued with Loc- Corresponding fracture values were indicated by FR400, FRV, and FRB,
tite Super Glue (Henkel Corp., USA) along these sides into a pack- with FR values determined in Rockwell indentations being basic
age, which was polished over the planes formed by their ground ones.
surfaces (3  25 mm2). This package was unglued in an acetone bath.
The experiments were carried out with an independent Ceram- 3. Results
Test device (Gobor Ltd., Ukraine) mounted on a universal test ma-
chine. The speed of the machine cross-head was constant and Experimental results are summarized in Table 2, and several
equal to 0.5 mm/min. The test specimens were glued to photo- fracture resistancefracture distance relations are presented in
graphic glasses with Loctite Super Glue and clamped on the XY Fig. 2. During investigation emphasis was placed not only on infor-
table of this device. mation of fracture resistance of glasses but also on the specic fea-
The tests made use of a standard diamond C-Scale Rockwell in- tures of fracture processes.
denter3 (200 lm tip radius), a conical indenter, being the modica- Indentation tests with a Rockwell indenter and a conical inden-
tion of a Rockwell indenter, with a 400 lm tip radius, as well as ter were performed to demonstrate that the tip radius of the rst
diamond Vickers and Berkovich pyramids. Vickers indenters were one is sufcient to consider it as an indenter corresponding to that
manufactured by Vilson Instruments (USA), other indenters were used in Hertzian indentations [20]. These resulted (Fig. 3) in prac-
made by Gilmore Diamond Tools, Inc. (USA). tically identical Hertzian surface ring cracks generated by a sphere
The studies were carried out in two stages. The fracture behav- [1]. Then surface cracks in the glass specimen, formed with a Rock-
ior of glass surfaces was rst studied by moving indenters from the
central zone of the specimen surface to its edge, then the behavior
of those edges was investigated with evaluation of glass ability to
resist fracture, i.e., the procedure was the same as in earlier studies
on ceramic materials.
During the experiments the indentation point on the specimen
surface was chosen by a magnifying glass, with PC registration of

2
It contains silicon, sodium, potassium, barium, cerium, neodymium, tungsten,
praseodymium, and oxygen.
3
The fracture of such a brittle material as glass is not inuenced by the conical
portion of the indenter. Fig. 1. Schematic measurement of the fracture distance L (KI fused silica).

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75 (a) 1 75 (b)
1

Fracture load Pf, N

Fracture load Pf, N


50 3
50

2
25 25 2
3

0 0
0.1 0.2 0.3 0.1 0.2 0.3
Fracture distance L, mm Fracture distance L, mm

Fig. 2. The FR L relation for neodymium (a) and TF-2 (b) glasses: Rockwell (1), Vickers (2), and Berkovich (3) indentations.

Fig. 3. Hertzian ring crack on a KI fused silica specimen surface fractured with Rockwell (a) and conical (400-lm tip radius) (b) indenters.

Fig. 4. Cracks on specimen surfaces of KI fused silica in Rockwell indentations (a) and of oat glass in Berkovich indentations (b).

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Fig. 5. Typical chip scars on KI fused silica (a, b, c) and oat glass (d, e, f): Rockwell (a, d) Vickers (b, e), and Berkovich (c, f) indenters.

well indenter approaching its edge, were examined. As seen in (Fig. 5(a), (d)). Quarz glass, in contrast to the above, can also dis-
Fig. 4(a), two additional, about diametrically opposite secondary play such chip scars in Vickers indentations [11]. These test results
cracks develop (primary crack is a Hertzian ring crack shown in that are within the scope of experimental contact mechanics also
Fig. 3), which then curve to the specimen edge. With further move- conrm that the EF method can be used without any limitations
ment of the indenter, these cracks come out at the specimen edge. for studying so-called anomalous glasses [24] (e.g., quartz glasses),
Then the chip separates from its body when the contact point of which do not exhibit cracks in Vickers indentations (Fig. 6(a)). The
the indenter approaches closer the specimen edge. And the chip above results are rather useful for better understanding the behav-
scar on the side surface acquires the form of a Hertzian quasi-cone ior of glasses and other brittle materials in edge aking.
[21]. Secondary cracks continue growing till no less than a half of Preliminary SEVNB tests (fracture of a V-notch bar in exure) of
the ring crack is formed, then only fragments of ring cracks develop examined glasses that we earlier used in all similar studies re-
without additional cracking (Fig. 5(a)). This fracture behavior of sulted in KIc = 0.60.9 MPa m1/2, which is consistent with data
glasses is probably consistent with the little studied Hertzian quar- [1]. But for the avoidance of testing the additional specimens in
ter-space problem [22]. comparative fracture toughness evaluation the IF method [19]
When a Vickers indenter moves to the specimen edge, cracks was applied (Table 2).
near imprint angles parallel to this edge, as in conical indentations,
curve along its direction (see also [23]). As opposed to this, cracks 4. Discussion
near a Berkovich imprint propagate to the specimen edge without
curving (Fig. 4(b)). Conical indentations of glass specimens usually As analysis of test data demonstrates (Table 2), oat glass re-
result in chip scars in the form of quasi-cones on their side surfaces sists fracture somewhat better than fused silica (higher FR values).

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Fig. 6. Vickers imprint on KI fused silica (a) and oat glass (b) specimen surfaces.

The fracture behavior of neodymium glass is similar to that of ical of ceramic materials (dark circles in Fig. 7). If this fact is ac-
fused silica. Notice that this behavior of examined glasses does counted for in fracture resistance calculations, FR values for 89
not depend on their silica content, which is close to 100% in KI, (open circles) and 48 (dark circles) chip scars would be 260 45
>70% in oat glass, 50% in F-2 int, and <40% in TF-4 heavy int. and 148 28 N/mm, respectively. These values are greatly differ-
As was expected [11], with an increase in stress concentrations ent from the average one for all chip scars (Table 2). Data-points
(linear contact zone of an indenter with the specimen surface), obtained in conical and Rockwell indentations can be equivalent
fracture resistance (FRV) values were smaller than FR values for fused silica tests (crosses and open circles in Fig. 7).
(Fig. 2 and Table 2), FRB values, corresponding to the point contact The structure of other glasses, containing atoms of different
zone of the indenter with the specimen surface, turned out to be modiers and intermediates, is inhomogeneous at the nanoscale
even lower (Fig. 2(a) and Table 2). However, the results of studying because no continuous siliconoxygen tetrahedral network would
the edge fracture of int and heavy int specimens in Berkovich occur in them. For instance, in glasses, containing lead oxide, Pb2+
indentations were quite unexpected (Fig. 2b): their FRB values are ions can be built in the tetrahedral network and occupy the verti-
higher than those of other glasses and higher than FRV values. This ces of PbO4 pyramids, which linked with siliconoxygen tetrahe-
effect is still unclear, but as is known, lead (Pb2+) can change elastic dra. Since the PbO bond is relatively weak due to the low eld
properties of glasses [25]. strength of very large Pb2+ ions [26], the network can be easily dis-
If the EF behavior of glass is viewed at the atomic scale (it does rupted. Though such glasses may have a higher or a lower fracture
not matter that the material has no long-range order and no peri- resistance, the scatter in their test data is much smaller (Fig. 2),
odic structure), interesting observations can be made. For example, probably, due to their lower sensitivity to above defects that is also
fused silica, being a three-dimensional network of corner con- typical of brittle composite materials. However, for nal conclu-
nected SiO4/2 tetrahedra [25], can be treated as a comparatively sions, additional studies would be necessary.
homogeneous material, but, as all glasses, contains such defects, Finally, it should be mentioned that for conventional elastic
as broken chains, structural inhomogeneities, microscale bubles, ceramics, fracture resistance to fracture toughness ratio can be
etc. Its test results exhibit a wide scatter of data when specimens about 100 times higher (without account of value dimensions)
are fractured under spherical contact, this phenomenon is not ob- [10]. If it is much higher, they are characterized by the EF barrier
served in point contact. Notice that only this glass displays two to the onset of fracture [10], as is seen, e.g., from the comparison
patterns of chip scars: conventional quasi-cones formed on the of data in Table 2. A similar ratio was also found in glass tests
side specimen surface (open circles in Fig. 7) and scallop-like typ- according to other versions of fracture resistance evaluation of
ceramics in edge aking (e.g., 261 N/mm [27]). It may be suggested
150 that a higher barrier to the onset of fracture is typical of all glasses
and can be considered as their specic feature. Hereinafter, it
would be appropriate to study its physical nature since just this
barrier may control the suitability of glasses in many applications.
The above also emphasizes that evaluation of glasses by their KIc
Fracture load Pf, N

100 values cannot be considered as adequate since fracture toughness


can characterize only the resistance of the material to the propaga-
tion of a preformed crack [28].

50
5. Conclusion

Comparative studies on the ability of different glasses to resist


the aking of their specimen edges by conical indenters with 200
0 and 400 lm tip radii, as well as by Vickers and Berkovich pyramids
0.1 0.2 0.3 0.4 0.5 have been carried out. It has been established that normal glass is
Fracture distance L, mm less subjected to fracture in spherical contact, while lead glass is
Fig. 7. Fracture diagrams of KI fused silica: data-points for quasi-cone chip scars (s
less fractured in point contact. The changes in glass behavior when
Rockwell and  conical indenters) and for scallop-like chip scars (d Rockwell a Rockwell indenter moves from the central specimen area to its
indenter) with approximating lines. edge have been followed. It is shown that in this case a Hertzian

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conical crack is transformed into a quasi-cone. It has been con- [9] G.A. Gogotsi, Mater. Res. Innovations 102 (2006) 179.
[10] G.A. Gogotsi, Strength of Mater. 38 (2006) 261.
rmed that glasses exhibit a higher resistance to initial fracture
[11] G.A. Gogotsi, S.P. Mudrik, Ceram. Int. 35 (2009) 1871.
with a blunt indenter than conventional ceramic materials. It has [12] G.A. Gogotsi, V.I. Galenko, S.P. Mudrik, B.I. Ozersky, V.V. Khvorostyany, T.A.
been demonstrated that the new approach to studying the fracture Khristevich, J. Eur. Ceram. Soc. doi:10.1016/j.jeurceramsoc.2009.12.002.
behavior of glasses is quite promising for practical applications. [13] G.A. Gogotsi, Ceram. Int. 35 (2009) 1109.
[14] G.A. Gogotsi, Ceram. Int. 35 (2009) 2735.
The EF test method can be employed to advantage in a normal [15] G.A. Gogotsi, V.I. Galenko, S.P. Mudrik, B.I. Ozersky, V.V. Khvorostyany, T.A.
materials science laboratory since it does not require any special Khristevich, Ceram. Int. 36 (2010) 345.
equipment and can be performed on small-size specimens. [16] GOST 15130-86, Silica optical glass, General specications, 1986 (in Russian).
[17] GOST 3659-78, Colourless optical glass, Physicochemical characteristics, Basic
parameters, 1978 (in Russian).
Acknowledgment [18] ISO 14705, Fine Ceramics (advanced ceramics, advanced technical ceramics)
Test Method for Hardness of Monolithic Ceramics at Room Temperature,
Switzerland, 2008.
The authors are thankful to Dr. T.I. Falkovskaya (KPI, Ukraine) [19] G.R. Anstis, P. Chantikul, B.R. Lawn, D.B. Marshall, J. Am. Ceram. Soc. 64 (1981)
for optical glasses used in experiments. 533.
[20] A.G. Evance, T.R. Wilshaw, Acta Metall. 24 (1976) 939.
[21] G.A. Gogotsi, V.I. Galenko, S.P. Mudrik, B.I. Ozersky, V.V. Khvorostyany, T.A.
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