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Long - term

Mechanical Properties
Stress Relaxation

Stress relaxation is defined as a


gradual decrease in stress with time,
under a constant deformation (strain).

This characteristic behaviour of the


polymers is studied by applying a fixed
amount of deformation to a specimen
and measuring the load required to
maintain it as a function of time.

This is in contrast to creep


measurement, where a fixed amount
Diagram illustrating stress relaxation.
of load is applied to a specimen and
resulting deformation is measured as
a function of time.
Stress Relaxation...

Stress relaxation behaviour of the polymers has


been overlooked by many design engineers and
researchers, partly because the creep data are
much easier to obtain and is readily available.

However, many practical applications dictate the


use of stress relaxation data.

For example, extremely low stress relaxation is desired


in the case of a threaded bottle closure, which may be
under constant strain for a long period. If the plastic
material used in the closures shows an excessive
decrease in stress under this constant deformation, the
closures will eventually fail.

Similar problems can be encountered with metal


inserts in molded plastics, Belleville washer, also
known as a coned-disc spring or multiple cantilever
springs used in cameras, appliances and business
machines.
Stress Relaxation...

Stress relaxation measurements can be carried


out using a tensile testing machine. However,
the use of such a machine is not always
practical because the stress relaxation test ties
up the machine for a long period of time.

The equipment for a stress relaxation test


must be capable of measuring very small
elongation accurately, even when applied at
high speeds.

Many sophisticated pieces of equipment now


employ a strain gauge or a differential
transformer along with a chart recorder
capable of plotting stress as a function of time.
Stress Relaxation...

A typical stress–time curve is


schematically plotted in Figure. At
the beginning of the experiment,
the strain is applied to the specimen
at a constant rate to achieve the
desired elongation.

Once the specimen reaches the


desired elongation, the strain is held
constant for a predetermined
amount of time.

The stress decay, which occurs


because of stress relaxation, is
observed as a function of time.
Stress–time curve.
Stress Relaxation...

If a chart recorder is not


available, the stress values at
different time intervals are
recorded and the results are
plotted to obtain a stress versus
time curve.

One such stress relaxation


curve plotted at various levels of
constant strain is shown in
Figure.

Stress relaxation curve plotted at various


levels of constant strain.
Stress Relaxation...

The stress relaxation experiment is often


carried out at various levels of temperature
and strain.

The stress data obtained from the stress


relaxation experiment can be converted to a
more meaningful apparent modulus data by
simply dividing stress at a particular time by
the applied strain.

The curve may be replotted to represent


apparent modulus as a function of time.

The use of logarithmic coordinates further


simplifies the stress relaxation data by allowing
us to use standard extrapolation methods such
as the one used in creep experiments.
Thermal Properties
Thermal Properties

The thermal properties of plastic materials are equally as important


as the mechanical properties.

Unlike metals, plastics are extremely sensitive to changes in


temperature.

The mechanical, electrical, or chemical properties of plastics cannot


be examined without looking at the temperature at which the values
were derived.

Crystallinity has a number of important effects upon the thermal


properties of a polymer. Its most general effects are the introduction
of a sharp melting point and the stiffening of thermal mechanical
properties.

Amorphous plastics, in contrast, have a gradual softening range.


Thermal Properties...
Molecular orientation also has a significant
effect on thermal properties. Orientation tends
to decrease dimensional stability at higher
temperatures.

The molecular weight of the polymer affects


the low-temperature flexibility and brittleness.

Many other factors, such as intermolecular


bonding, cross linking, and copolymerization, all
have a considerable effect on thermal
properties.

Hence, it is clear that the thermal behaviour of


polymeric materials is rather complex.

Therefore, in designing a plastic part or


selecting a plastic material from the available
thermal property data, one must thoroughly
understand the short term as well as the long-
term effects of temperature on the properties
of that plastic material.
Thermal Properties...

Tests for elevated temperature performance

Designers and material selectors of plastic products


constantly face the challenge of selecting a suitable plastic for
elevated temperature performance. The difficulty arises
because of the varying natures and capabilities of various
types and grades of plastics at elevated temperatures.

Many factors are considered when selecting a plastic for a


high-temperature application.
i) The material must be able to support a design
load under operating conditions without objectionable creep
or distortion.
ii) The material must not degrade or lose necessary
additives that will cause a drastic reduction in the physical
properties during the expected service life.
Tests for elevated temperature performance... Thermal Properties...

All the properties of plastic materials are not


affected in a similar manner by elevating
temperature. For example, electrical properties
of a particular plastic may show only a
moderate change at elevate temperatures,
while the mechanical properties may be
reduced significantly.

Thus, it is quite clear that a single maximum-


use temperature that will apply to all the
important properties in high-temperature
applications is simply not possible.
Tests for elevated temperature performance... Thermal Properties...

When studying the performance of plastics at elevated temperatures,


one of the most important considerations is the dependence of key
properties such as modulus, strength, chemical resistance, and
environmental resistance on time.

Therefore, the short-term heat resistance data alone is not adequate


for designing and selecting materials that require long-term heat
resistance.

For the sake of convenience and simplicity, we divide the elevated


temperature effects into two categories:

1. Short-term effects 2. Long-term effects


a. Heat deflection temperature a. Long-term heat resistance test
b.Vicat softening temperature b. UL temperature index
c. Torsion pendulum c. Creep modulus/creep rupture
tests
Tests for elevated temperature performance... Thermal Properties...

Short-Term Effects
A. Heat Deflection Temperature (HDT) (ASTM D 648, ISO 75-1 & 75-2)

Heat deflection temperature is defined as the temperature


at which a standard test bar (5 × 1/2 × 1/4 in.) deflects
0.010 in. under a stated load of either 66 or 264 psi.

The heat deflection temperature test, also referred to as


the heat distortion temperature test, is commonly used
for quality control and for screening and ranking materials
for short-term heat resistance.

Heat distortion temperature, however, does distinguish


between those materials that lose their rigidity over a
narrow temperature range and those that are able to
sustain light loads at high temperatures
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

Apparatus
The apparatus for measuring heat deflection temperature consists of an
enclosed oil bath fitted with a heating chamber and automatic heating
controls that raise the temperature of the heat transfer fluid at a uniform
rate.

A cooling system is also incorporated to fast cool the heat transfer medium
for conducting repeated tests.

The specimens are supported on steel supports that are 4 in. apart, with the
load applied on top of the specimen vertically and midway between the
supports.

The contact edges of the support and of the piece by which pressure is
applied is rounded to a radius of 1/4 in.

A suitable deflection measurement device, such as a dial indicator, is normally


used. A mercury thermometer is used for measuring temperature. The unit is
capable of applying 66- or 264-psi fiber stress on specimens by means of a
dead weight.
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

A commercially available heat


deflection measuring device with a
closeup of a specimen holder is
illustrated in Figure
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

Test Specimens

The test specimens consist of test bars 5 in. in length


and 1/2 in. in depth by any width from 1/8 to 1/2 in.

The test bars may be molded or cut from extruded


sheet as long as they have smooth, flat surfaces and are
free of excessive sink marks or flash.

The specimens are conditioned employing standard


conditioning procedures.
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

Test Procedure.

The specimen is positioned in the apparatus along with


the temperature and deflection measuring devices and the
entire assembly is submerged into the oil bath kept at
room temperature.

The load is applied to a desired value(66- or 264-psi fiber


stress).

Five minutes after applying the load, the pointer is


adjusted to zero and the oil is heated at the rate of 2 ±
0.2°C/min.

The temperature of the oil at which the bar has deflected


0.010 in. is recorded as the heat deflection temperature at
the specified fiber stress.
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

Factors Influencing HDT

• Residual Stress. The specimens consisting of a high degree of


“molded-in” residual stresses or a high degree of orientation
have a tendency to stress relieve as the temperature is
increased. The specimen warpage occurs in a downward
direction owing to the external loading. The warpage due
to stress relaxation and deflection, occurring from the
softening of the specimen, combined together, yields a false
heat deflection temperature.

However, if the specimens are annealed in a controlled


oven atmosphere prior to testing, the stresses can be
relieved and warpage can practically be eliminated. Heat
deflection temperature of the unannealed specimen is
usually lower than that for a comparable annealed
specimen.
Short-Term Effects
A. Heat Deflection Temperature (HDT) ... Thermal Properties...

Factors Influencing HDT


Specimen Thickness.
Thicker specimens tend to exhibit a
higher heat deflection temperature.
This is because of the inherently low Fiber Stress. The higher the fiber
thermal conductivity of plastic stress or loading is, the lower the
materials. The thicker specimen heat deflection temperature. The
requires a longer time to heat difference in heat deflection
through, yielding a higher heat temperature values resulting from
deflection temperature. different fiber stress varies
depending upon the type of
polymer.

Specimen Preparation.
Injection-molded specimens tend to have a
lower heat deflection temperature than
compression-molded specimens. This is
because compression-molded specimens are
relatively stress-free.
Thermal Properties...
Short-Term Effects
B. Vicat Softening Temperature (ASTM D 1525, ISO 306)

The Vicat softening temperature is the temperature at


which a flat-ended needle of 1-mm2 circular cross
section will penetrate a thermoplastic specimen to a
depth of 1 mm under a specified load using a
selected uniform rate of temperature rise.

This test is very similar to the deflection temperature


under the load test and its usefulness is limited to
quality control, development, and characterization of
materials.

The data obtained from this test is also useful in


comparing the heat-softening qualities of
thermoplastic materials.

However, the test is not recommended for flexible


PVC or other materials with a wide Vicat softening
range.
Short-Term Effects Thermal Properties...
Vicat Softening Temperature (ASTM D 1525, ISO 306)...

The test apparatus designed for


deflection temperature under load
test can be used for the Vicat
softening temperature test with
minor modification.

The flat test specimen is molded or The test is carried out by first
cut from a sheet with a minimum placing the test specimen on a
thickness and width of 0.12 and 0.50 specimen support and lowering the
in., respectively. needle rod so that the needle rests on
the surface of the specimen.

The temperature of the bath is raised


at the rate of 50 or 120°C/hr
uniformly.

The temperature at which the needle


penetrates 1 mm is noted and
reported at the Vicat softening
temperature.
Short-Term Effects Thermal Properties...
Vicat Softening Temperature (ASTM D 1525, ISO 306)...

A commercially
available test
apparatus for
measuring the Vicat
softening
temperature is
illustrated in Figure

Vicat softening point apparatus.


Thermal Properties...

Long-Term Effects

During long-term exposure to heat, plastic materials may


encounter many physical and chemical changes.

A plastic material that shows little or no effect at elevated


temperature for a short time may show a drastic
reduction in physical properties, a complete loss of rigidity,
and severe thermal degradation when exposed to elevated
temperature for a long time.

Along with time and temperature, many other factors such


as ozone, oxygen, sunlight, and pollution combine to
accelerate the attack on plastics.

At elevated temperatures, many plastics tend to lose


important additives such as plasticizers and stabilizers,
causing plastics to become brittle or soft and sticky.
Thermal Properties...
Long-Term Effects

Three basic tests have been developed and accepted by the


plastics industry.

If the application does not require the product to be exposed


to elevated temperature for a long period under continuous
load, a simple heat-resistance test is adequate.

The applications requiring the product to be under


continuous significant load must be looked at from creep
modulus and creep rupture strength test data.

Another widely accepted method of measuring maximum


continuous use temperature has been developed by
Underwriters Laboratories.

The UL temperature index, established for a variety of plastic


materials to be used in electrical applications, is the
maximum temperature that the material may be subject to
without fear of premature thermal degradation.
Thermal Properties...
Long-Term Effects
A. Long-Term Heat-Resistance Test (ASTM D 794)

The long-term heat-resistance test was


developed to determine the permanent effect
of heat on any property by selection of an
appropriate test method and specimen.

In ASTM recommended practice, only the


procedure for heat exposure is specified and
not the test method or specimen.
Thermal Properties...
Long-Term Effects
A. Long-Term Heat-Resistance Test (ASTM D 794)

Any specimen, including sheet, laminate, test bar, or molded


part may be used.

If a specific property, such as tensile strength loss is to be


determined, a standard tensile test bar specimen and
procedures must be used for comparison of test results
before and after the test.

The test requires the use of a mechanical convection oven


with a specimen rack of suitable design to allow air
circulation around the specimens. The test is carried out by
simply placing the specimen in the oven at a desired
exposure temperature for a predetermined length of time.
Thermal Properties...
Long-Term Effects
A. Long-Term Heat-Resistance Test (ASTM D 794)

The subsequent exposure to temperatures may be increased


or decreased in steps of 25°C until a failure is observed.

Failure due to heat is defined as a change in appearance,


weight, dimension, or other properties that alter plastic
material to a degree that it is no longer acceptable for the
service in question.

Failure may result from blistering, cracking, loss of plasticizer,


or other volatile material that may cause embrittlement,
shrinkage, or change in desirable electrical or mechanical
properties.
Thermal Properties...
Long-Term Effects
A. Long-Term Heat-Resistance Test (ASTM D 794)

Many factors affect the reproducibility of the data.

The degree of temperature control in the oven, the


type of molding, cure, air velocity over the
specimen, period of exposure, and humidity of the
oven room are some of these factors.

The amount and type of volatiles in the molded


part or specimen may also affect the reproducibility.
Thermal Properties...
Long-Term Effects
B. Creep Modulus/Creep Rupture Tests

The tests developed to determine creep


modulus and creep rupture values of plastic
materials are discussed earlier.

Both creep modulus and creep rupture


strength decrease significantly as the
temperature is increased.

Before selecting a material for a load-bearing


application at an elevated temperature, one
must carefully evaluate the published creep
modulus and creep rupture strength test data.
This is accomplished by using bar charts.
Thermal Properties...
Long-Term Effects
B. Creep Modulus/Creep Rupture Tests

In one chart, creep


modulus of various
thermoplastics at three
different temperatures is
compared.

Creep modulus versus temperature.


Thermal Properties...
Long-Term Effects
B. Creep Modulus/Creep Rupture Tests

A similar comparison is made


using creep rupture strength
for the same set of
thermoplastic materials.

A study of the charts reveals


that while most of these
thermoplastics have
substantial rigidity and
strength at room
temperature, only a few retain
enough of these properties at
elevated temperatures to bear
significant loads

Creep rupture strength versus temperature.