Report
No. GL-99-2
LINKS This
report contains links to outside resources and documents that are
pertinent to the context of the information in this report.
The following list will take you to the point in the report
where you can use each link:
CWC
(formerly the Clean Washington Center) NIST
Manufacturing Extension Service The
Pacific Northwest Economic Region (PNWER) U.S.
EPA A
report describing the fusing process A
manufacturer of fused glass tile A
procedure for finding the densest packing
of particles A
manufacturer of rock tumblers for mixing materials A
manufacturer of glass kilns A
manufacturer of electronic controllers for kilns A
manufacturer of glass processing systems The
American Society for Testing and Materials A
manufacturer of strength testing equipment A typical composition of soda lime glass
TABLE OF CONTENTS
Page INTRODUCTION.................................................................................................................... 1 1.0 GLASS CHARACTERISTICS........................................................................................ 2 1.1 Glass..................................................................................................................... 2 1.1.1 Previous work with Recycled Glass..................................................................... 2 2.0 SAMPLE TILE PRODUCTION...................................................................................... 4 2.1 Standard Mix Ingredients....................................................................................... 4 2.1.1 Glass................................................................................................................... 4 2.1.2 Binder................................................................................................................ 4 2.1.3 Water................................................................................................................ 5 2.1.4 Salt.................................................................................................................... 5 2.2 Standard Mixing Processes............................................................................................ 5 2.3 Standard Firing.............................................................................................................. 7 2.4 Mix Variations............................................................................................................... 8 2.4.1 Variation of the Glass Component....................................................................... 8 2.4.2 Variation of the Binder Component................................................................... 10 2.4.3 Variation of the Water Component................................................................... 10 2.4.4 Variations in Firing Processes........................................................................... 11 2.4.5 Other Variations............................................................................................... 11 3.0 TESTING AND TEST METHODS...............................................................................
12 3.1 Compression Testing................................................................................................... 12 3.1.1 Procedures...................................................................................................... 13 3.2 Flexure Testing............................................................................................................ 14 3.2.1 Procedures...................................................................................................... 15 3.3 Absorption Testing...................................................................................................... 20
4.0 SAMPLE STRENGTH AND ABSORPTION PROPERTIES.................................... 21 4.1 Effect of Position in Kiln............................................................................................. 21 4.2 Effect of Kiln Firing Temperature................................................................................ 22 4.3 Effect of Kiln Type..................................................................................................... 25 4.4 Effect of Particle Size Gradation.................................................................................. 25 4.5 Effect of Glass Color.................................................................................................. 27 4.6 Other Types of Tile.................................................................................................... 28 4.7 Effect of Coloring Agent............................................................................................. 28 4.8 Effect of Water Content.............................................................................................. 28 4.9 Green Strength........................................................................................................... 28 4.10 Compressive Strengths.............................................................................................. 29 4.11 Flexural vs. Compressive Testing............................................................................... 29 4.12 Flexural Strength-Compressive Strength Relationship................................................. 30 4.13 Effect of Addition of Inorganic Binder #3................................................................... 32 4.14 Effect of Mix and Amount of Binder Material............................................................. 32 4.15 Absorption................................................................................................................ 34 4.16 Statistical Variation of Strength and Absorption.......................................................... 34 5.0 IMPLICATIONS OF TILE PERFORMANCE FOR APPLICATION....................... 35 6.0 CONCLUSIONS.............................................................................................................
35 7.0 REFERENCES................................................................................................................ 38
LIST OF FIGURES Figure
1 - Kiln Temperature History.............................................................................................
7 Figure
2 - Typical Grain Size Distribution.....................................................................................
9 Figure
3 - Third Point Loading Method for Flexural Testing of Samples...................................... 16 Figure
4 - Specimen Under Load...............................................................................................
18 Figure
5 - Stacking Test (Batches 11-16)...................................................................................
22 Figure
6 - Stacking Test (Batch 20)...........................................................................................
23 Figure
7 - Strength vs. Maximum Kiln Temperature....................................................................
24 Figure
8 - Average Absorption vs. Maximum Kiln Temperature for Standard
Kiln...................... 24 Figure
9 - Average Strength vs. Number of Particle Gradations for Fondu.................................. 26 Figure
10 - Average Absorption
vs. Number of Particle Gradations for Fondu ..........................
27 Figure
11 - Average Flexural
Strength for Test Batches.............................................................
31 Figure
12 - Average Percent Absorption
for Test Batches.........................................................
31 Figure
13 - Average Strength
vs. Percent Binder.......................................................................
33 Figure
14 - Absorption Over Time
...........................................................................................
33 APPENDICES APPENDIX
A: Table 1 - Production
Parameters APPENDIX
B: Table 2
- Physical
Characteristics of Residual Fibers
INTRODUCTION Post-consumer
recycled glass collections have grown faster than the infrastructure
that exists to use it. Therefore,
the development of alternative uses for post-consumer recycled
glass is critical to the economic viability of an increasing number
of recycling programs. This project tested glass and inorganic binder
paver tiles made from mixed-color recycled glass for strength
and absorption in order to assess the tiles' fitness for use.
This report: ·
gives
some background information on previous research done on recycled
glass tiles; ·
describes
methods used in the production of the recycled glass tiles tested
in this study; ·
describes
the tests performed on the tiles; ·
gives
the results of the tests; and ·
discusses
implications of the study for potential production. 1.0 GLASS CHARACTERISTICS 1.1 GLASS The
tensile strength of glass rods or fibers drawn in a vacuum may
be as high as 6200MPa (900,000psi), and plate glasses may have
strengths as high as 173MPa (25,000psi).
The tensile strength of ordinary soda lime glass is usually about 70MPa (10,000psi).
However, sand blasted glass, in which many flaws have been
created, has a strength of only 14MPa (2000psi).
These data demonstrate that highly polished and flawless
glass has much higher tensile strength than glass with surface
flaws. Fracture mechanics has demonstrated that surface
flaws concentrate stress, causing failures at lower tension than
would be expected with flawless surfaces.
This phenomenon is mentioned because the samples tested
during this project have body composition very close to solid
glass. It will be demonstrated that the tensile strength
of these materials approach that of solid glass which has been
sandblasted.
The
modulus of elasticity of the glass is in the vicinity of 65,500MPa
(10,000ksi), which is approximately one-third that of steel and
three times that of normal strength portland cement concrete.
(Cordon, 1979 and Felbeck and Atkins, 1984). 1.1.1 Previous work with Recycled Glass Previous
work with recycled glass has involved the development of processes
for manufacturing paving or mosaic tiles from sintered recycled
glass. Brown and MacKenzie (1982) used powdered glass
and up to 10% clay binder to form a composite material. Clay binder was necessary to give a “green”
strength for transfer to the kiln before final firing. It was found that green strength was affected
by the amount of clay binder, particle size, pressing pressure
and amount of water. Fired
strength was shown to be considerably greater than that of commercial
clay based tiles. Higher stiffness and strength were obtained
with smaller particles, less water and binder, and greater pressing
pressure. Pressing pressure
ranged from 10MPa (1500psi) to 40MPa (5800psi).
Binder content ranged from 4% to 20%.
Kiln heating rates of between 100º
C/hr and 350º C/hr
(180º-630º
F/hr) gave essentially the same properties, while lower rates
resulted in lower strength and stiffness.
Slow cooling was important.
The strength and stiffness of the samples was greatest
when the peak kiln temperature was between 920° C and 950º
C (1688º F -1742º F). The maximum modulus
of rupture was found to be approximately 4.8x106kg/m2
(47.1MPa; 6800psi).
The
making of mosaic glass from ground waste glass is described by
Liu, Li, and Zhang (1991). They
used several types of chemical binder to produce mosaic glass
of the required texture. The glass was formed into samples and sintered
by firing at 640° C - 800º
C (1,184° F - 1,472º
F) for 30 minutes before slow cooling.
The tiles fired at temperatures of 720ºC
(1,328º F) had bending
strengths which were 1.90-3.22 times stronger than those fired
at 640º C (1,184º F), and that strength tended to increase with firing temperature.
The maximum bending strength obtained was 10.56kg/cm2
(1.04MPa or 150psi). Specimens fired at 640º C (1,184º F) had water
absorption of up to 5.25%, while those fired at temperatures at
least 720º C (1,328º F) had no appreciable absorption.
In
contrast with both of the projects above, this project tested
tiles made without pressing.
Rather, shaking or tapping the molds was used to obtain adequate density before
firing. The CWC has published
other reports on
the process of sintering glass without binders in open molds.
There are manufacturers of glass tiles using these methods.
2.0 SAMPLE
Tile Production Much
of the work was accomplished by using a standard mix to make a
standard test tile with approximate fired dimensions of 14"
x 4" x 1". The approximate fired weight was 1850g.
2.1 STANDARD MIX INGREDIENTS 2.1.1 Glass The
glass component was a combination of coarse and fine particle
gradations. In this report, the terms coarse and fine designate
particle size with reference to a US#200 sieve. Fine particles pass through a US#200 sieve,
whereas coarse particles are retained on this sieve. For the standard mix, only one range of coarse glass particle sizes
was used. These particles
passed through a US#6 sieve and were retained on a US#16 sieve. The notation “A x B” is used to mean particles
passing a US#A sieve and retained on a US#B sieve. The coarse component is therefore described
as 6x16. The fines are
described as "collector dust," which are a waste resulting
from the manufacture of plate or “flat” glass.
The coarse component was green, while the fines from the
plate glass were clear. All of the glass was of the soda-lime variety.
2.1.2 Binder The
tiles included a small amount of inorganic binder. The amount added was 2.7% by weight of the glass component. The glass component in the standard mix was
1800 grams. Inorganic
Binder #1 (IB1) was 2% by weight of glass, or 72g, and the inorganic
binder #2 (IB2) was 0.7%, or 13g.
The
binder gave the specimens enough green strength after drying to
allow handling after being removed from the mold.
This enabled the mold to be removed before the kiln firing. Therefore, the mold can be made from any material
that can withstand a 200º
F drying chamber. Additionally,
the refractory nature of the inorganic binder helped the material
to maintain its shape during the firing process.
Although the glass component gave the material its fired
strength, the binder also effects the sintering process.
Therefore, the fired strength was influenced by the amount
and type of binder. Specifically,
the binder can inhibit the sintering process.
A balance is required between the amount of binder needed
for workability (for green strength and to maintain specimen shape
during firing) and the amount that will severely diminish the
fired strength.
2.1.3 Water To
achieve the desired consistency of the mixture, a quantity of
water was added. The quantity
of water added in the standard mix procedure was 250 grams; this
equaled 13.9% by weight of the glass.
2.1.4 Salt The
addition of a small amount of a salt helped to reduce the tendency
of the water to “pool” on the surface of the material in the mold. The salt acted as a “deflocculant,” which inhibited the clumping
of the smaller particles, kept them in suspension, and enabled
the water to be held within the material as it was leveled in
the mold. The result was a better mixture between coarse
and fine particles, which increased the particle packing efficiency.
2.2 STANDARD MIXING PROCESS The
production process was designed to be as uncomplicated and reproducible
as possible. Much of the
process involved readily available and non-specialized tools and
equipment.
More
closely packed particles reduce shrinkage and produce a stronger
fired product. Thus, it
was desirable to find the combination of coarse and fine particles
that would yield the densest packing of the two gradations.
The 3 to 1 ratio of coarse to fine particles was arrived
at in the following manner. Maintaining
a total mass of 400 g, various combinations of coarse and fine
(e.g. 350 coarse, 50 fine; 325 coarse, 75 fine) particles were
mixed and placed in a long graduated tube with an internal diameter
of 1 inch (25.4 mm).
The tube itself was then raised and tapped down 200 times
from a height of 2 inches onto a piece of foam-backed carpet.
The combination of coarse and fine glass that tapped down
the most was found to be the 300g coarse and 100g. Respectively, the particle packing efficiency
was then estimated using a specific gravity for glass of 2.5. Knowing the volume occupied by the mixture
(from the graduated tube) and the mass (fixed at 400g), a bulk
density, rbulk, of the mixture was calculated
and compared to the density of solid glass, rglass. The particle packing
efficiency, defined as rbulk/rglass, for this combination of fines and coarse
gradations was 60%.
Initially,
the two gradations of glass particles, coarse and fine, were measured
in a 3 to 1 ratio; 1350 g of coarse and 450 g fine glass. The powdered binder consisted of
2% by weight or 72g of inorganic binder #1 and 0.7% by weight or 13g of inorganic binder #2.
The
three dry ingredients were mixed in a rock tumbler. The water to be added, 13.9 % by weight or 250 g, was then measured.
One-quarter teaspoon of a salt was mixed into the water
using a standard kitchen blender. The water/salt mixture was then added to the
dry ingredients in a bowl and mixed by hand.
After
all of the ingredients had been mixed, they were placed in a mold
on a shaker table.
The mold was lightly lubricated with vegetable shortening
to ease “demolding.” The table was then activated and the material
settled in the mold. The
top surface of the specimen was smoothed using a common paint
scraper. Brown et al (1982) showed that increasing the
pressing pressure on the material from 10MPa (1.450psi) to 40
MPa (5800psi) produced a 14% increase in fired strength.
However, the process under consideration required only
vibratory compaction under gravity.
2.3 STANDARD FIRING The
mold and material were placed in the kiln and dried at 150° F (66° C) for ten hours. The
lid of the kiln was left open during drying. After drying, the specimen had enough strength,
referred to as “green strength”, to be handled. After the specimen was removed from the mold,
it was returned to the kiln.
Firing the tiles involved heating them to a peak temperature
of 1600° F (871° C), holding for one hour, and cooling. Figure 1 shows the temperature history. The temperature within the kiln was controlled
by using an
The
firing temperature was chosen to cause the glass particles to fuse
by heating and bonding without melting.
The goal was to achieve a fired body that would not absorb
water and have high strength, a process called sintering.
The sintering temperature is several hundred degrees less
than the temperature required to fully melt the glass but some softening
does occur, as described by Shackelford (1992) below: “The
material...is formed by the densification of a powder. The bonding of powder particles occurs by solid-state
diffusion. In the course
of this densification stage, the pores between adjacent particles
steadily shrink. This overall process is known as sintering.
The mechanism of shrinkage is the diffusion of atoms away
from the grain boundary (between adjacent particles) to the pore.
In effect, the pore is “filled in” by diffusing material.”
(Shackelford, p.298). The
kiln used to fire our test samples was oval shaped (plan view) and
27 inches deep. Up to six
shelves could be stacked vertically, and each shelf contained a
number of specimens.
2.4 MIX VARIATIONS For
a full description of the production parameters for all the test
specimens, see Appendix A, Table 1.
Note that the parameters which differ from the standard mix
are shown in bold face. The last column of the table indicates the
variable that was being examined for each batch.
2.4.1 Variation
of the Glass Component As
glass was the largest component of the tiles, much of the experimentation
involved variation in the color of glass, the coarse/fine ratio
and the size-gradation of the coarse particles.
The
glass color for the coarse component of each batch is given in the
third column of Table 1. The
colors used for the coarse component included green, clear, amber
and mixed. Mixed color glass in this case is referred
to as “Andela” glass because it was processed in an Andela Glass Processing System. The number of different gradations is given
in the fourth column. The
fines were generally clear glass, although amber fines were substituted
for some batches.
Some
important batch differences:
·
In the
production of Batches 3 and 20, mixed color Andela glass with a
gradation of “#8 minus” (all of the particles passed a US#8 sieve)
was used as the coarse component.
The hole size of the US#8 sieve was 2.36 mm.
A typical grain size distribution for Andela glass is shown
in Figure 2.6. ·
Batch
20 also included a coarser component; this one designated as 3/8
x 1/8 (particles had a grain size of between 3/8 in and 1/8 in). ·
Batches
4 and 23 used a higher percentage of fines.
·
Batches
6, 18, 23 and 25 used clear glass instead of green for the coarse
particles. ·
The “pure
glass” specimens (Batches 8, 10, 17 nd 27) were made with green
glass of gradation “16minus” (all particles passed a US#16 sieve).
A typical grain size distribution for the glass component
of the "pure glass" specimens is shown in Figure 2.
2.4.2 Variation of the Binder Component ·
Calcium
aluminate cement (“fondu”) was used as the binder in Batches 5,
7, 24 and 28.
·
The amount
of added fondu ranged from 6.3% for Batch 28 to 10% for Batch 24.
·
The binder
type and the percent by weight (of the glass component) for each
batch can be found in columns 5 and 6 of Table 1.
·
In addition,
specimens were made that contained no binder (Batches 8, 10, 17
and 27). These batches are
referred to as “pure glass” specimens and were fired in a mold. This required a mold that was resistant to kiln temperatures.
2.4.3 Variation of the Water Component ·
Generally,
the amount of water added equaled 250g.
·
However,
260g was used in Batch 4 to obtain the required consistency in the
mixture with the finer glass. Because
of the greater surface area-to-volume ratio of the finer particles
in Batch 4, it was not surprising that more water was needed to
achieve the same consistency.
·
No water
was added to the pure glass specimens.
·
For the
samples which used fondu as the binder, differing amounts of water
were added.
·
Batches
5, 7 and 24 used 300 g and Batch 28 contained specimens with 250
g, 275 g and 300 g of added water.
·
Table
1, column 7 shows the quantity of water used for each batch.
2.4.4 Variations in Firing Process ·
While
1600°F (871° C) was the standard maximum kiln temperature, specimens in
Batches 9 and 10, Batches 2 and 8, Batches 18 and 19, and Batches
25-27, were fired at maximum kiln temperatures of 1400°F (760° C), 1500°F (816° C), 1650°F (899° C) and 1700°F (927° C), respectively. When
the maximum kiln temperature was altered, the rate of temperature
change was also adjusted so that the duration of the peak temperature
phase remained constant at one hour.
·
The maximum
kiln temperature used for a given batch is found in column 8 of
Table 1, Appendix A. ·
Two different
kilns were used to fire the tiles.
A common, oval-shaped pottery kiln was used for the majority
of the tiles, but a standard rectangular “flat” kiln was used for
Batches 29-34.
·
The type
of kiln used in the production of a given batch is shown in column
9 of Table 1, Appendix A.
2.4.5 Other Variations ·
Several
batches included certain additives.
·
A metal
oxide stain was used as a coloring agent to make Batch 33. The amount added was only 0.25% by weight of
the glass component.
·
In addition
to the fondu binder, inorganic Binder #3 (IB3) was added to Batch
28. 3.0 Testing
and Test Methods 3.1 COMPRESSION TESTING There
is no standard or code which describes compression testing of glass
paving tiles. However, ASTM C67 (1992) “Standard Test Methods of Sampling
and Testing Brick and Structural Clay Tile” provides a method which
is applicable to glass.
The
test procedure involves capping the specimen (at least 5 inches
(127 mm) in diameter) with either gypsum or sulfur-filler.
The tile is then placed flat on the test machine, centered
below the spherical head mounted block.
Compressive force is applied at a uniform rate in order to
move from one-half the peak load to the peak load in one to two
minutes.
Other
test procedures are given for masonry units in ASTM C140, “Standard
Methods of Sampling and Testing Concrete Masonry Units”.
A sample aspect ratio (height-to-width ratio) of two is specified.
The
minimum required compressive strength of a paving brick subjected
to light traffic is given in ASTM C902 (1982) “Standard Specification
for Pedestrian and Light Traffic Paving Brick."
It is 8000psi for an average of five bricks, or 7000psi for
an individual brick that will be subject to the most severe environment
--- where the brick may be frozen while wet.
Average strengths of 3000psi and individual strengths of
2500psi are acceptable in less severe environments.
The
paving tiles described in this report were relatively flat, therefore
it was difficult to obtain the aspect ratio of 2:1 required by ASTM
C140. Therefore, ASTM C67 was more appropriate for
testing, however, it was not considered to be fully appropriate
for the following reasons:
·
the code
is material specific (written for brick and clay but not for glass); ·
it specifies
capping using various methods for brick and clay. These methods are not necessarily appropriate
for glass tiles; and ·
there
is no reference to the required aspect ratio of the specimens. Different aspect ratios would be expected to
produce different strengths. For
example, confining effects at the center of a tall thin specimen,
due to the end plates restraint, will be less than that on a short
squat specimen. The shorter specimen would therefore be expected
to be stronger. 3.1.1 Procedures The
compression tests were accomplished by using a Baldwin, 300 kip (1335kN) capacity testing machine.
The compression testing was performed on disks approximately
one inch thick (25.4mm) and having a diameter of about 3.7 inches
(94mm). The diameter was
measured from each face of the disk using a caliper gauge with a
readability of +/- 0.01 in (0.25mm).
The area used in calculating the stress was found by averaging
the diameter measured on each load bearing face of the specimen
according to ASTM C67, 6.4.1.
The
upper bearing block of the machine was larger than the specimen
itself. If the opposite were true (the upper block
smaller than the specimen) it is expected that during the loading,
some confining pressure would be exerted by the surrounding material
on the material being directly loaded.
This would tend to increase the maximum load able to be sustained
by the specimen.
In
general, the specimens that were tested had some unevenness on the
load-bearing faces. The
face that was cast face-up was particularly rough.
Several methods were attempted to avoid stress concentrations
and early failure due to the uneven surface of the compression specimens.
The first method involved using a neoprene pad on the roughest
surface and nothing on the other face.
This technique was discarded because of concern that the
neoprene layer, which tended to “bulge-up” around the sides of the
specimen, could exert some confining pressure and thus postpone
the failure of the specimen. Not enough tests were performed using the pad
to assess the validity of this concern.
In
order that the load bearing faces are even and parallel, the ASTM
standard described techniques for “capping” the specimens. Without any sort of capping scheme, it was expected that the applied
load could be unevenly distributed and concentrated on the higher
points of the specimen. Therefore,
the portion of the total cross-sectional area that was being directly
loaded would fail first. Thus,
the maximum load and average compressive stress, calculated as the
maximum load over the total area, would be less than if the entire
specimen were bearing the load evenly.
Strengths
obtained showed that there was little difference in compressive
behavior between specimens that had been capped and those which
had not. Therefore, in order to facilitate testing,
no cap was used. By not
capping the specimens, the maximum load capacity should be underpredicted. 3.2 FLEXURE TESTING Using
a third-point loading on a beam, which has a depth equal to one-third
of the span, is a method of flexural testing and is described in
ASTM C78 (1984), “Flexural Strength of Concrete.”
In this type of loading, the specimen is supported at the
ends and two equal loads are applied, such that the specimen is
sectioned into thirds. This produces a constant bending moment over
the middle third of the span. “Third-point”
loading is depicted in Figure 3.
A
flexure test for a thinner specimen, such as the ones used in this
study, is described in "Sampling
and Testing Brick and Structural Clay Tile" (ASTM C67). However, this standard prescribes a centerpoint loading. Here, one load is applied at the center of
the span. There is no specification for the minimum
modulus of rupture required for paving tiles.
3.2.1 Procedures The
flexural (bending) tests were carried out using a Baldwin, 60 kip
capacity testing machine. Figure
4 shows the testing apparatus.
The method used in this study did not rigorously conform
to either ASTM procedure because the “third point” method of loading
was used and the tiles were much shallower than ASTM C78 concrete
beams. The recycled glass specimens tested in this report have a
depth of approximately 1/12 the span.
However, there is no theoretical difference in the way that
flexural tension stress, given by the Modulus of Rupture, was calculated
for a “shallow” beam, as compared to a “deep” beam.
The depth of a particular specimen used should not matter,
as it is accounted for in the Modulus of Rupture formula.
The modulus of rupture may be computed in the following ways
based on the standard beam elastic formulae. Figure 3. Third Point Loading Method for Flexural Testing of Samples
B) Free Body Diagram (specimen)
For
the third-point loading scheme:
PL where: P
=
maximum load (lb) bd2 b = specimen width (in) For the centerpoint loading
scheme:
where: d
= specimen depth (in)
3Pa P = maximum load (lb)
bd2
d = specimen
depth (in)
a = average
distance from
failure plane to end
support (in)
The
specimens used in this test were relatively flat, rectangular
tiles. The length was approximately 14.25 inches (362mm)
and the clear span was 12 inches (305mm). The width was approximately 4 inches (102mm) and depth was approximately
one inch (2.54 cm). They were tested using a third-point loading
technique, which was designed to create an equal maximum bending
moment over the entire middle third of the span.
Thus, failure was expected to occur in this portion of
the specimen. If it occurs
too far outside of the middle span, the test result is probably
affected by a weakness in the region of lower moment.
Failures within 5% of the total span length outside the
middle third are permitted by the ASTM.
For the 12 inch (305mm) span used, this equals almost 5/8
in (15.9mm). All specimens
tested failed in the region of maximum moment.
The
following is the test procedure used.
The specimen is first labeled and marked (using a ruler)
at 4 inch (102mm) centers to show division into thirds.
Next, the specimen is positioned on the support bars, such
that the end marks lie over the steel bars, with the inch or so
protrusion extending past the contact point of the bars.
These supports form a 12 inch (305mm) span.
The upper bearing plate has spherically seated bars 4 inches
(102mm) apart. It is positioned over the two center marks
and the entire setup is centered under the testing machine head. The load is applied at the prescribed rate
of less than 2000 lb/min (8918 N/min), according to ASTM C 67,
until failure occurs. The
maximumload registered by the testing machine is recorded.
After
failure, the measurements of the width and depth of the specimen
cross-section are made at the two ends and along the edge of failure
. The width measurement is made at mid-height
of the cross sections and the height is taken along the centerline
of the specimen. In the
case where there are two failure planes, one is arbitrarily chosen
at which to measure. From these values, an average width and height
are calculated. These
average values are used to calculate the modulus of rupture.
The
specimens used had a slight taper of approximately 5° around the edges of the upper surface,
sometimes more noticeable along one edge of the specimen than
the other. This taper was ignored in the measurement of
the dimensions. Thus,
the calculated value of the Modulus of Rupture was slightly conservative.
Because
of the taper, the contact area of the specimen with the upper
bars may have been less
than it would have been if the upper surface was perfectly flat.
This resulted in the applied load not being as evenly distributed
and thus higher stress concentrations in certain regions of the
specimen during loading. This effect was considered small and was ignored.
Another
aspect of the test method was the weight of the upper bearing
plate, which was positioned over the specimen and transferred
the load from the testing machine.
The weight of the entire apparatus (one plate, two bars
and two balls) equaled 30.2 lb (134.7 N). For a specimen to be able to bear a substantially
greater load, such as a deeper beam, the effect of this weight
on the modulus of rupture calculation would be negligible. However, for the shallow specimens used, this
amounted to about 4% of the maximum load registered by the machine. The weight of the apparatus was considered
in the calculation of the Modulus of Rupture of the specimens.
Furthermore,
the weight of the specimen itself (about 4 pounds) creates a distributed
load over the length of the specimen and contributes to the theoretical
maximum bending moment. This
weight is ignored in the calculation.
Including it would add approximately 10psi, or 0.4% of
the peak strength, to the modulus of rupture values.
Ignoring it, as we have chosen to do, makes the obtained
result more conservative. 3.3 ABSORPTION TESTING Absorption
testing was carried out instead of specific freeze thaw testing
according to ASTM C67, section 7.3.2.1.
According
to ASTM C67, the pieces were first dried in an oven at a temperature
of about 230°F (110°C) for a 24 hour period. They
were allowed to cool to room temperature and weighed. This weight was recorded as the dry weight
W(d) .
Next, they were immersed in a tank of water at approximately
room temperature and left to soak for a 24 hour period. They were removed from the water and blotted dry to remove surface
water until they were no longer “shiny,” and weighed again to
get the saturated weight, W(s). The weight of water absorbed divided by the
dry weight equals the percent absorption:
%absorption = W(s) - W(d) where: W(s) = saturated weight W(d) For
this test, pieces of tiles that had previously been broken in
the flexure tests were used.
This is in accordance with ASTM C 67: “The specimens for
the absorption test shall consist of ... tile or ... representative
pieces from each of these...”
However,
the ASTM standard made no specific mention of what size pieces
were to be used. As specimens
of a constant thickness get smaller, the specific surface (the
ratio of surface area-to-volume) gets larger.
Theoretically, this could influence the amount of absorption,
as greater specific surfaces have greater portions of the material
directly exposed to the immersion bath. In
order to facilitate testing,
there was some experimentation with modifying the ASTM
C67 procedure. It was found that generally, the weight “as
is” (prior to any oven drying), was almost exactly the same as
the weight after oven drying.
Thus, some initial tests were carried out using no drying
phase at all. However,
because of concerns with potential questions about the testing
methods used and to assure validity of the results, it was resolved
to strictly adhere to the prescribed guidelines. The
absorption limit for paving brick in the most severe environment
is 8%, according to ASTM C902 (1992). 4.0 Sample
Strength and Absorption Properties Testing
was performed on a variety of specimens to investigate the relationship
between performance and production parameters.
A summary of the results of all the specimens tested is
given in Appendix B, Table 2 and referenced by batch number. 4.1 EFFECT OF POSITION IN KILN An
early concern in the project was that the kiln temperature might
vary throughout the depth of the kiln, causing the fired properties
of the tiles to be affected by their position.
This was investigated in the “stacking test” (Batches 11-16). In this test, specimens prepared with the same specifications were
fired in a kiln having vertically stacked shelves. There were six shelves stacked in the kiln,
each with three specimens. After
the testing of all the fired specimens was complete, an average
strength was calculated for each shelf.
No relationship was discovered between the
position in the kiln and the fired strength. Average strength versus kiln position is shown for Batches 11-16
in Figure 5.
Similar
results were found for specimens in Batch 20.
These specimens were fired in a kiln with three vertically
stacked shelves, each shelf having three specimens.
An average strength was calculated for each shelf. Again, no dependency on kiln position was discovered,
as shown in Figure 6.
4.2 EFFECT OF KILN FIRING TEMPERATURE The
maximum kiln firing temperature ranged from 1400°F (760°C) to 1700°F (927°C). The maximum temperature
used to fire each batch can be found in Appendix A, Table 1, column 8. For
the standard mix specimens, Batches 1, 2, 9, 11-16, 19 and 26,
and the pure glass specimens, Batches 8, 10, 17 and 27, the fired
strength initially increased as the maximum kiln temperature increased,
as shown in Figure 7. However, the strength for both peaked at 1600°F (871°C ) and then started to decline as maximum kiln temperature
continued to increase. In
Figure 7 the standard mix results at 1600°F are based
on the average results of Batches 1 and 11-16.
For
the standard mix, the absorption properties also exhibited temperature
dependency. Initially,
the absorption decreased as the maximum temperature increased. This was followed by a slight increase in absorption as the temperature
continued to increase past 1650° F (899° C), as shown in Figure
8.
It appears that at a critical
temperature, in the range of 1600°F-1650°F (871°C-899°C), optimal particle sintering occurs for
the standard mix and pure glass specimens.
This
gives the fired material greater density (fewer voids), which
improves the strength and decreases the amount of absorption.
This behavior was also observed by Brown et al. (1982). The specimens fired at 1500°F (760°C) tended to shatter into several pieces in the flexure test,
whereas, the 1600°F (871°C) specimens exhibited a “cleaner” failure
with a unique failure plane and little debris.
The
physical appearance of the pure glass specimens changed with temperature. Batch 17, fired at 1600°F (871°C), actually looked less glassy (more matte) than Batch 10,
which was fired at 1400°F (760°C). This
is possibly due to devitrification occurring at
the
higher temperature. The
large increase in fired strength between the 1500°F (816°C) and 1600°F (871°C) pure glass specimens indicates that a critical sintering
temperature exists in this range.
The
absorption of the pure glass specimens (Batch 17) fired at 1400°F (760°C) was less than for the 1600°F (871°C) batch (Batch
10). This behavior was
opposite to trends seen in the standard mix, showing higher absorption
at lower firing temperatures.
This can be attributed to the fact that the absorption
in either case is less than 0.1 %, and within this very small
range, the data may not be entirely reliable. It was found during the testing that the absorption
of the pure glass specimens could be reduced to almost zero through
extra surface drying. The
strength of the clear glass, Batches 6, 18 and 25, tended to increase
with firing temperature as shown in Figure 7.
4.3 EFFECT OF KILN TYPE The
majority of the specimens tested were fired in the aforementioned
“oval” kiln. Another type
of kiln, a “flat” kiln, was also used in making some of the tiles. In order to determine the influence of kiln type on fired behavior,
samples made with the standard mix were fired at the usual temperature
in the flat kiln (Batch 32).
The performance of these specimens were found to be 1.4%
less than that of the standard-mix specimens fired in the oval
kiln, as shown in Appendix B, Table 2.
As this difference was small, it seems reasonable to discount
any effects the flat kiln may have had on the fired properties.
4.4 EFFECT
OF PARTICLE SIZE GRADATION
A
comparison was made between specimens prepared using glass with
only coarse particles and those which had both coarse and fine
particles. Batch 5 was made with 1300 g of coarse glass.
Batch 7 was made with 1150 g of coarse glass and 150 g
of fine glass. The total
mass was the same for both. The
specimens in Batch 7 were made with two particle size gradations;
these were expected to have higher packing and fewer voids.
Strength
was 21% greater and the absorption was 47% less for the batch
that used a mix of two different particle sizes (Batch 7), rather
than a single gradation (Batch 5).
These results are shown in Figures 9 and 10.
A mixture of both coarse and fine particles resulted in a denser and stronger
fired specimen.
For
the two Andela batches, strengths from Batch 20 with 2 gradations,
were less than those from Batch 3 with 3 gradations.
However, this may have resulted from an unfavorable mixing
ratio of the gradations involved -- an insufficient number of
medium-sized particles may have lessened the surface contact and
sintering with the largest particles.
Visually, the specimens in Batch 20 were “blobby” and did
not appear to have packed and bonded well.
4.5 EFFECT OF GLASS COLOR The
results for the different glass colors are shown in Figure 7. At 1600°F (871°C), specimens
made using green glass for the coarse particles were 53% stronger
than those using clear glass.
The maximum strength for clear glass occurred at a kiln
temperature of equal or greater than 1700°F (927°C), while that for green glass occurred
at a temperature of 1600°F (871°C). Clear
glass contains less coloring agents than green or amber glass.
Coloring agents or additives tend to decrease the softening
temperature of the glass. Therefore, at low kiln temperatures, less sintering of the clear
glass takes place so it is weaker than colored glass. Because of kiln limitation, no testing was performed on clear glass
specimens fired at temperatures higher than 1700°F, so it was not possible to state whether
or not the strength versus temperature curve for clear glass would
peak at some critical temperature.
The strongest Andela tiles, Batch 3, were 6% stronger than
the average for the standard mix batches.
4.6 OTHER TYPES OF TILE An
assessment was made of the properties of some commercially available
brick and tile. Batch
21, made of clay, and Batch 22, made of concrete, were subjected
to flexural and absorption testing. The dimensions of these samples were smaller
than could be accommodated by the third-point test method, so
they were tested under centerpoint loading.
The modulus of rupture was about one-half that of the standard
mix. The absorption of the commercial tiles was
between 4% and 6%, which was worse than the 0.25% for the standard
mix.
4.7 EFFECT OF COLORING AGENT An
eventual production goal is to produce recycled glass tiles in
a variety of colors. In
order to test the effect of a coloring agent on performance, Batch
33 was prepared using the standard mix with a small amount (5g,
which is 0.28% of the glass weight) of metal oxide stain.
It was found that this reduced the fired strength of the
tiles to 19% below that of the standard mix. The absorption did not change significantly
4.8 EFECT OF WATER CONTENT There
was variation of the water content within Batch 28. There were three specimens made with 250g of water, one specimen
with 275g and one with 300g.
The results did not reveal a performance trend.
The 275g specimen was weaker than both the 250g specimens
and the 300g specimen (see results for Batch 28, Appendix A, Table
1). Additionally, the numbers of samples were too
small to draw any statistical conclusions; more investigation
is needed in this area.
4.9 GREEN STRENGTH The
modulus of rupture of the pre-fired green material was not able
to be computed accurately, as the tiles broke under the weight
of the loading apparatus. This caused a modulus of rupture of approximately
100psi. However, the green
strength was sufficient for production in all cases, as the green
specimens could be removed from the mold and handled without breaking.
4.10 COMPRESSIVE STRENGTHS Average
compressive strengths obtained for samples with a firing temperature
of 1600°F (871°C) were in the 24.5 to 27 ksi (169 to 186 MPa) range. This is much higher than typical strengths
of concrete cylinders, with a height-to-diameter ratio of 2:1,
which range from 3ksi to 8ksi (20.7MPa to 55.2MPa).
It is also higher than the 8ksi (55.2MPa) required for
tiles by ASTM C 902. Test samples used in this study were “flat”
-- they had a height to diameter ratio of about 0.25. Specimens with lower height-to-diameter ratios generally have higher
strength than those with greater height-to-diameter ratios, as
a result of end confinement.
This may be one reason for the high strengths.
However, ASTM C 902 does not specify required height-to-diameter
ratios for the tests. As
obtained strengths clearly surpassed 8000psi (55.2MPa), the glass
tiles satisfy this code requirement.
Compressive strength of Batch 9, fired at 1400°F (760°C) was about half that of the specimens
fired at 1600°F (871°C). 4.11 FLEXURAL VS. COMPRESSIVE TESTING Although
a compression test is specified in the minimum standard requirements
for pavers and minimum compressive strength cited, it seems that
compressive strength may not be as valuable a performance parameter
as flexural strength. This is acknowledged by ASTM: “It is the consensus...that
compressive strength does not truly express a significant property
of a paving unit. Rather,
a flexural property...will be more meaningful.“ (ASTM C 936). ASTM further states that a specification value
for a tensile strength test has not yet been determined.
The
validity of compression testing for the flatish tiles is called
into question as the specimens “failure” was not registered by
the testing machine until well after serious cracking and crushing
of the specimen occurred.
Failure
is most likely to occur if a paver is insufficiently supported. The loading creates a situation much like the
one emulated by the flexure test.
Failure would be expected to occur in flexure before compression
failure occurred. For
this reason, more tension tests than compression tests were carried
out.
While
a standard for the performance of a flexural strength test for
brick and structural clay tile does exist in ASTM C 67, no mention
is made of a minimum required flexural strength.
ASTM C 902 states only that “Minimum modulus of rupture
values should be considered by the purchaser for uses of brick
where support or loading may be severe.” 4.12 FLEXURAL STRENGTH-COMPRESSIVE STRENGTH RELATIONSHIP An
often-used rule of thumb is that the modulus of rupture of concrete
is approximately 10% of the compressive strength (Derucher, p.107). For the glass tiles tested, the ratio of the tensile strength to
the compressive strength was also approximately 1:10. The results of all the flexure tests are summarized in Figure 11.
The strengths of the commercial tiles, Batches 21 and 22,
and also Batch 9, which was made by firing at 1400°F (760°C), were about one-half that of the other batches. Batches 17 and 27, made from pure glass with
no binder, were significantly stronger than the others.
Most
tiles had moduli of rupture ranging from 1500psi to 3000psi. There is no minimum value of modulus of rupture
given in the standards. However,
if the relationship between compressive strength and modulus of
rupture of 10:1 is used, then a modulus of rupture of 800psi (5.5MPa)
would relate to a compressive strength of 8000psi (55.2MPa). All of the samples tested have moduli of rupture
greater than 800psi (5.5MPa), so they should be satisfactory for
use as paving tiles.
Batches
24 and 28 show the effect of the addition of inorganic binder
#3 (IB3). Batch 28, which contained 100 g of inorganic
binder #3 (5.6% of glass weight) had an absorption of 3.9%, while
Batch 24, which contained no inorganic binder #3, had an absorption
of 3.0%. The strength was not diminished; in fact, it
was slightly higher (4.2%) for the batch containing inorganic
binder #3. 4.14 EFFECT OF MIX AND AMOUNT OF BINDER MATERIAL In
the standard mix, the binder was 2% inorganic binder #1 and 0.7%
inorganic binder #2. A
comparison of the results of Batch 29, where the binder is inorganic
binder #1 only, with those from Batch 30 containing inorganic
binders #1 and #2, show that this small amount of inorganic binder
#2 is important. Batch
29 made with 2% inorganic binder #1 as binder had lower strength
than Batch 30 specimens, which used 2% inorganic binder #1 and
0.7% inorganic binder #2. Increasing
the amount of binder had very noticeable effects. Batch 31 was made with the standard mix, except that the amount
of binder was raised to 3.7% (3% inorganic binder #1 and 0.7%
inorganic binder #2), instead of the usual 2.7%.
The strength of this batch was 26% less than the average
for all the standard-mix specimens.
Increasing the binder level to 4.7% resulted in an even
larger reduction in strength of 32%, relative to the standard-mix
average. The strength
of the strongest fondu tiles, Batch 7, was 81% of the standard
mix average. The
specimens made with no binder had the highest fired strength and
lowest absorption of all of the tiles tested.
Figure 13 shows how strength varied with percentage binder
for the standard mix specimens.
The
results from the absorption tests show that the material made
from recycled glass had low absorption.
Figure 12 summarizes the absorption test results.
The values obtained were all quite low, generally less
than 1% (or approaching zero absorption).
These were well below the most severe allowable values
of 8% for brick given in ASTM
C902, “Standard Specification for Pedestrian and Light
Traffic Paving Brick.” High
absorption was obtained from the commercial bricks (Batches 21
and 22), as well as by those tiles made with the fondu binder
(Batches 5, 7, 24 and 28). The
addition of inorganic binder #3 increased the absorption of the
tiles, as shown by comparing Batches 24 and 28.
It would be expected that tiles with high absorption would
be the most susceptible to freeze-thaw damage.
The
absorption test requires immersion over a 24 hour period. When carried out over a prolonged duration,
the measured percentage of absorption did not show a marked increase. Figure 14 shows these results.
4.16 STATISTICAL VARIATION OF STRENGTH AND ABSORPTION The
standard deviations of the strengths were generally low, as given
in Appendix B, Table 2. For
example, for the Batch 1 flexural tests, the standard deviation
was 155psi (1.07MPa), which was 6% of the average strength of
2573psi (17.7MPa). For
other batches, the standard deviation was generally less than
10% of the average value. This
scatter was low considering that recycled glass is a brittle material
in which fracture may be initiated by any small imperfection.
The scatter for absorption was generally significantly
greater. For example, the standard deviation was 20%
of the average value for Batch 1.
It is thought that scatter was high because the absorptions
were low and were difficult to measure accurately, as explained
previously. 5.0 IMPLICATIONS OF TILE PERFORMANCE
FOR APPLICATION The
previous chapter has shown that the strength and absorption properties
of well made recycled glass tiles is as good as, and often much
better than, ASTM requirements for similar types of material.
The significance of the difference in strength between
concrete and glass tiles is described below. In
the testing which was undertaken, the modulus of rupture of the
glass tiles was often more than two times that of the commercial
clay and brick tiles. While there is likely to be a wide variation
in strength of commercial clay and brick tiles made by different
manufacturers and different methods, it is assumed in this discussion
that the ratio of modulus of rupture of glass tiles to that of
concrete tiles is about two. It
was shown in Section 3 that the modulus of rupture of a material
is related to the thickness of the tile squared.
Therefore, the required thickness of glass tiles is 1/Ö2 (or 0.71) times that of concrete tiles,
in order for them to carry the same load.
For example, if it were desired to produce a glass tile
with a bending resistance equivalent to that of a one inch
(25.4mm) thick concrete tile, then a 0.71in (18mm) thick
glass paving tile would be required.
Also, a concrete tile having the same bending resistance
as a one inch (25.4mm) thick glass tile would have to be 1.41in
(35.9mm) thick.
6.0 Conclusions A
number of recycled glass paving tile test samples were manufactured
using low technology procedures.
Proportions of raw material and production process parameters
were altered. The performance of the tiles was assessed in
terms of their flexural strength, compressive strength and absorption
capacity. It was found
that:
Compressive
strength: Average compressive strengths ranged from 14
- 27 ksi (96MPa -186Mpa). This
is much greater than the most severe ASTM requirement of 8ksi
(55MPa). Generally the specimens were not capped. Flexure vs. Compression: Modulus
of rupture rather than compressive strength was shown to be a
better parameter to estimate tile performance.
Flexural Strength: Flexural
tests gave moduli of rupture ranging from 1156psi (7.97MPa) to
4483psi (30.9MPa). Average
modulus of rupture was 6% to 11% of the compressive strength. The required compressive strength of 8,000psi (ASTM C 902) conservatively
relates to a modulus of rupture of 800psi. All tiles tested were therefore satisfactory.
Effect
of Binder on Strength: Strengths of samples increased with lower amounts
of binder. Addition of
small amounts of inorganic binder #3 increased the absorption,
but had little effect on the strength.
Tiles made with fondu binder were weaker than those made
with the standard mix. Effect of Particle Gradation
on Strength: Strength generally increased with a wider difference
between the particle gradations.
Effect of Glass Color on Strength: Clear glass had a higher sintering temperature
than green or amber glass. This
caused the strength of clear glass to be lower than colored glass
at kiln temperatures less than about 1675 °F (913 °C), and greater
at higher temperatures. Green
and amber glass behaved similarly, however only one batch of amber
tiles was tested. Effect of Kiln Temperature
on Strength: Strengths of “standard samples” made with green
glass increased with increasing kiln temperature up to a temperature
of 1600 °F (871 °C); thereafter, strength declined. Effect of Kiln Type and Position: Behavior of the tiles was not affected by the
position of the tiles in the kiln, or the type of kiln used.
Behavior of Commercial Brick
and Concrete Tiles: Average modulus of rupture of the commercial
brick and concrete tiles tested were 1356psi (9.35MPa) and 1053psi
(7.26MPa), respectively. This
is significantly less than the modulus of rupture of the standard
glass tile of 2677psi (18.46MPa).
Design of Glass Tiles: As
recycled glass tiles have a greater modulus of rupture than concrete
tiles, the same bending resistance may be obtained with a thinner
tile.
Absorption: Absorption
of water in glass tiles was generally less than 1%. Clay and concrete tiles showed an absorption
of 4-5%, and tiles made with a fondu (calcium aluminate cement)
as binder had absorptions from 1- 4%.
The lowest absorptions occurred in tiles fired at 1650
°F ( 899°C). Lower absorptions were obtained from mixes
made from a wider range of particle gradation than those with
a narrow range of gradation.
Overall Performance: The
recycled glass tiles showed very good strength and absorption
properties without being overly sensitive to any of the mix or
production parameters. It
is believed that there is a lot of promise for the further production
and use of these tiles. 7.0 References
ASTM
C 78 - 84 (1984). Standard
Test Method for Flexural Strength of Concrete (Using
Simple Beam with Third-Point Loading).
ASTM
C 67 - 92a (1992). Standard
Test Methods of Sampling and Testing Brick and Structural Clay
Tile.
ASTM
C 293 - 79 (1979). Standard
Test Method for Flexural Strength of Concrete (Using Beam With
Center-Point Loading).
ASTM
C 140 - 91 (1991). Standard
Methods of Sampling and Testing Concrete Masonry Units.
ASTM
C 902 - 92 (1992). Standard
Specification for Pedestrian and Light Traffic Paving Brick.
ASTM
E 4 - 93 (1993). Standard
Practices for Force Verification of Testing Machines.
Brown,
I.W.M. and K.J.D. Mackenzie, 1982.
Process design of a ceramic-like body from recycled
waste glass. Journal of Materials Science, pp. 2164-2193.
Derucher,
Kenneth N., George P. Korfiatis, A. Samer Ezeldin, 1994. Materials for Civil & Highway Engineers.
Grolier’s
Electronic Encyclopedia (1996).
Liu,
Wansheng, Shuzhen Li and Zhangying Zhang, 1991.
Sintered mosaic glass from ground waste glass.
Glass Technology, February.
Shackelford,
James F., 1992. Introduction
to Material Science for Engineers.
Macmillan.
Tauber,
E. and Crook, D.N., 1965. British
Clayworker, 74 (42)
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