"Pressure Sensitive Adhesive For Use in Nibration/Sound-Damping"
BACKGROUND OF THE PRESENT INVENTION
The present invention is directed to an ultra-clean pressure sensitive
adhesive composition for use in vibration/sound-damping.
A quiet operating environment is often highly desirable in the high
performance computer and PC gaming systems. Computer systems generally
include at least one or more disk drives for storage of information. Such disk
drives are generally in the form of a sealed head-disk assembly chamber which
includes one or more disks stacked on a spindle motor hub. The acoustic noise
of a disk drive arises from the spindle motor and disks ("Idle Acoustics") and
from the moving actuator that supports the read/write heads ("Seek
Acoustics"). On the other hand, during operation of the disk drives, vibration
at various frequencies also occurs as a result of the mechanical resonance of the
various components of the sealed head-disk assembly. It is thus desirable to.
provide means to damp vibration/sound resulting from operation of such
devices.
The problem of vibration/sound-damping is not, however, restricted to
computer systems. Such problems also exist in the automobile industry as
well as conventional appliances, as well as any other application requiring the
use of motors or related vibration or sound-inducing mechanisms.
Many attempts have been made to address this problem. See, for
example, U.S. Patent Nos. 4,942,187 (vibration-damping rubber composition of
hexene-1 type polymer and Si-containing graft copolymer and inorganic
reinforcing agent); 5,279,896 (mechanical design for disk drive vibration and
noise damping); 5,464,659 (vibration damping material comprised of acrylic
monomers, silicone adhesive, and optional crosslinker); 5,781,373 (soft metal
substrate for disk drive noise reduction); 5,858,521 (vibration damping material
of a laminate of a viscoelastic layer and a hardenable pressure sensitive
adhesive layer); 5,939,179 (vibration damping material comprised of one
surface of a rigid body and a polymer layer of synthetic rubber); and 6,216,817
(preparation of damping coating by photopolymerization); U.S. published
patent application No. 20010044023 (vibration attenuating article having a
non-tacky film covering substantially all of the article); and EP 390207
(vibration damping material comprised of blend of fluorine-containing polymer
and acrylic polymer). Such attempts have not always been successful. For
example, in the computer industry, any material used in connection with the
computer hardware must be low-volatile and non-corrosive in nature (i.e.,
ultra-clean). Conventional adhesives have not generally satisfied this
requirement. The adhesive material which is employed must also provide
vibration/sound-damping over a wide frequency range, possess both cold flow
and heat resistance, and provide high adhesion and good strippability.
OBJECTS AND SUMMARY OF THE PRESENT INVENTION
It is accordingly an object of the present invention to provide a pressure
sensitive adhesive composition that may be used in vibration/sound damping
applications.
It is also an object of the present invention to provide an ultra-clean
composition that exhibits pressure sensitive adhesive properties.
In accordance with the present invention , there is provided a pressure
sensitive adhesive comprised of the following:
(A) a copolymer comprised of the polymerization reaction product of an
alkyl (meth)acrylate monomer having a Tg > 20 °C, optionally a C1-3o
(meth)acrylate monomer, optionally a nitrogen-containing polar monomer, and
optionally a polymerizable epoxy-containing monomer, said monomers being
present in an amount such that the Tg of said copolymer (A) is greater than
about -2 °C; and
(B) a copolymer comprised of the polymerization reaction product of an
optional vinyl acetate or vinyl ether component, (C2-12) alkyl (meth)acrylate,
hydroxy(C1-5)alkyl(meth)acrylate, and optionally a polymerizable epoxy-
containing monomer, said monomers being present in an amount such that the
Tg of said copolymer (B) is less than about -20 °C, and
wherein said copolymers (A) and (B) are present in said composition in
a weight ratio ranging from about 0: 100 to about 40:60.
There is also provided a method of damping vibrations or sound in an
article comprising providing a film or layer of a vibration or sound damping
material to the article such that said film or layer is capable of attenuating said
vibration or sound in at least one vibrational or sound mode, the film or layer
being comprised of the above composition.
DETAILED DESCRIPTION OF THE PRESENT INVENTION
The adhesive composition of the present invention is comprised of low
Tg copolymer (B) either alone or together high Tg polymer (A) and which may
be used with particular advantage in vibration/sound-damping.
The composition of the present invention enables a number of benefits
to be achieved. For instance, the composition enables highly desirable
damping and absorption characteristics to be achieved over a wide freguency
range (1Hz to 10 kHz). The tan delta of the composition (measured by
Dynamic Mechanical Analysis) is an indication of energy loss and the
composition of the invention enables values above 0.6 (at 1Hz), 1.2 (at 100
Hz), 2.1 (at 1kHz) and 3.0 (at 10kHz) to be achieved (thus confirming the
ability of the composition to provide vibration/sound-damping).
Dynamic Mechanical Analysis (DMA) provides a useful tool to study
the dynamic properties of a material and is often used to characterize the sound
or vibration damping performance of polymers, particularly viscoelastic
polymers. The tan delta of the material, as defined by the ratio of Loss
Modulus (G) to Storage Modulus (G'), is a valuable indicator of the material's
relative damping ability. Any peak in tan delta (particularly apparent in
temperature profile studies) corresponds to a region where the material
properties are changing rapidly; i.e., the material is undergoing a transition. In
frequency dependent studies, a peak in tan delta indicates that the material
dissipates the incident sound or vibration energy and converts to heat very well
at that frequency. High values of tan delta over a wide range of frequency is
generally regarded as the platform for good broadband damping properties.
The composition of the present invention may be used with advantage
in the electronics industry as the composition may be tailored to be ultra-clean
by avoiding the presence of acid or polar components; i.e., the composition will
preferably exhibit a leachable ion concentration below 22 ng/cm2 , with
outgassing as measured by Dynamic Headspace Analysis using GC-MS below
910 ng/cm2. Such values are within the parameters of the hard disk drive
industry standards.
The demands on the electronics industry to increase memory capacity
are driving the improvements in cleanliness levels. The development of MR
(magnetoresistive) and GMR (giant magnetoresistivity) head technologies, with
recording heads floating over the memory surface on a molecular layer of air,
make trace amounts of VOC's (volatile organic compounds originating from
the adhesive) operate as miniature "speed bumps" when they condense on the
memory surface. This disrupts the reading and writing process, which is the
essence of the electronic data storage and retrieval process.
The composition of the present invention also, due to its crosslinkable
nature, may be crosslinked to exhibit inherent hardness, cold flow resistance,
heat resistance, and broad band vibration attenuation. By way of example, a
typical shear modulus (G') range measured by Dynamic Mechanical Analysis
is 5xl05 dyne/cm2 (at 1Hz), 2.1xl06 dyne/cm2 (at 100 Hz), 6.2 x 106 dyne/cm2
(at 1 kHz) and 2.6xl07 dyne/cm2 (at 10 kHz).
The composition of the present invention can be fine tuned to exhibit a
range of adhesion, as desired.
The composition of the present invention may be used to damp
vibrations or sound in an article by providing a film or layer of a vibration or
sound damping material to the article comprised of the composition such that
the film or layer is capable of attenuating vibration or sound in at least one
vibrational or sound mode. For example, the composition may be coated on a
surface of the article which surface is particulary related to the formation of
vibrations or sound.
The high Tg copolymer (A) used in the composition of the present
invention is comprised of the polymerization reaction product of an alkyl
(meth)acrylate monomer having a Tg >20 °C, optionally a C 1-30 (meth)acrylate
monomer, an optional nitrogen-containing polar monomer, and an optional
epoxy-containing monomer, each as defined below. The monomers are
present in an amount such that the Tg of the resulting polymer is greater than -2
°C.
The alkyl (meth)acrylate monomer having a Tg > 20 °C. may be
selected from but not limited to the group consisting of t-butyl (meth)acrylate,
hexadecyl acrylate, isobornyl (meth)acrylate, cyclododecyl acrylate, methyl
methacrylate, secondary butyl methacrylate, ethyl methacrylate, cyclohexyl
methacrylate and mixtures thereof.
The optional C1-30 (meth)acrylate monomer used in the present invention
may comprise a monomeric (meth)acrylic acid ester of a non-tertiary alcohol
wherein the alcohol portion has from 4 to 18 carbon atoms. Exemplary
(meth)acrylate monomers include but are not limited to esters of (meth)acrylic
acid with non-tertiary alcohols such as 1-butanol, 1-pentanol, 2-pentanol, 3-
pentanol, 2-methyl- 1-butanol, 1-methyl-pentanol, 2 -methyl- 1-pentanol, 3-
methyl- 1-pentanol, 2-ethyl-l-butanol, 3,5,5-trimethyl-l-hexanol, 3-heptanol, 2-
octanol, 1-decanol, 1-dodecanol, etc.
Exemplary monomeric (meth)acrylate monomers having a carbon chain
of at least 12 carbon atoms include but are not limited to lauryl acrylate (C12),
tridecylacrylate (C13), myristyl acrylate (C14), palmityl acrylate (C16) and
stearyl acrylate (C18). Such monomers are well-known to those skilled in the
art.
The at least one nitrogen-containing polar monomer may be selected
from a wide range of suitable monomers. Such monomers include, for
example, vinyl monomers having at least one nitrogen atom. Such monomers
include but are not limited to N-mono-substituted acrylamides, such as a
(meth)acrylamide, N-methylacrylamide, N-ethylacrylamide, N-
methylolacrylamide, N-hydroxyethylacrylamide and diacetone acrylamide;
N,N-disubstituted acrylamides such as N,N-dimethylacrylamide, N,N-
diethylacrylamide, N-ethyl-N-aminoethylacrylamide, N-ethyl-N-
hydroethylacrylamide, N,N-dimethylolacrylamide, and N,N-
dihydroxyethylacrylamide, etc.
Exemplary nitrogen-containing monomers may also include but are not
limited to N- vinyl lactam monomers such as N-vinyl-2-pyrrolidone, 5-methyl-
N-vinyl-2-pyrrolidone, 5-ethyl-N-vinyl-2-ρyrrolidone, 3 ,3-dimethyl-N-vinyl-2-
pyrrolidone, 3-methyl-N-vinyl-2-pyrrolidone, 3-ethyl-N-vinyl-2-pyrrolidone;
4-methol-N-vinyl-2-pyrrolidone; 4-ethyl-N-vinyl-2-pyrrolidone; N-vinyl-2-
valerolactam; N-vinyl-2-caprolactam; N-vinyl-2-piperidone; and N,N-
dimethylacrylamide and mixtures of any of the foregoing. The corresponding
allyl derivatives thereof are also suitable for use in the present invention. The
noted lactams may also be substituted in the lactam ring by one or more lower
alkyl groups having from 1 to 4 carbon atoms, with methyl; ethyl, or propyl
groups being particularly preferred. The N- vinyl lactam monomer employed
preferably comprises N-vinyl-2-pyrrolidone.
The polymerizable epoxy-containing monomer may be selected from a
variety of vinyl-terminated epoxy-containing monomers. Exemplary
polymerizable monomers include but are not limited to glycidyl esters of an
α,β-ethylenically unsaturated carboxylic acid, such as (meth)acrylic or
crotonoic acid.
Exemplary glycidyl monomers for use in the present invention
accordingly include but are not limited to glycidyl (meth)acrylate, glycidyl
ethacrylate and glycidyl itaconate, acryl glycidyl ether, (meth)allyl glycidyl
ether and 3,4-epoxy-l-vinylcyclohexane.
The alkyl (meth)acrylate monomer is present in the copolymerizable
reactant mixture in an amount ranging from about 20 to 80 percent by weight,
the polymerizable C1-3o (meth)acrylate monomer is present in the mixture in an
amount ranging from about 0 to 50 percent by weight, the nitrogen-containing
polar monomer is present in the mixture in an amount ranging from about 0 to
50 percent by weight, and the polymerizable epoxy-containing monomer is
present in the mixture in an amount ranging from about 0 to 50 percent by
weight. The epoxy-containing monomer is preferably present in an amount
greater than 15 percent by weight.
Other monomers in addition to the above monomers may be optionally
included for reasons such as cost reduction, etc. For example, styrene and
vinyl acetate may be incorporated into the copolymer with advantage. Such
monomers, if present, will be employed in amounts such that the resulting
copolymer will still have a Tg greater than 50 °C.
The alkyl (meth)methacrylate monomer is present together with the
nitrogen-containing monomer in an amount such that the resulting copolymer
exhibits a Tg > 50 °C, and preferably at least 60 °C. Copolymer (A) does not
inherently exhibit pressure sensitive adhesive properties. However, the
polymer finds particular utility when blended with low Tg copolymer (B) to
form a crosslinkable pressure sensitive adhesive composition.
Copolymer (B) a copolymer comprised of the polymerization reaction
product of an optional vinyl acetate or vinyl ether component, C(2-
12)alkyl(meth)acrylate, hydroxy(C1-s)alkyl(meth)acrylate, and an optional
polymerizable epoxy-containing monomer (defined in the same manner as
defined in connection with copolymer A). The monomers are present in an
amount such that the Tg of said copolymer (B) is less than about -20 °C.
Exemplary hydroxy(C1-5)alkyl(meth)acrylate monomers include but are
not limited to hydroxyethyl(meth)acrylate, hydroxypropyl(meth)acrylate,
hydroxybutyl(meth)acrylate, and corresponding dihydroxy compounds.
While a number of (C2-12)alkyl(meth)acrylate monomers may be
employed, the preferred monomer is 2-ethylhexylacrylate.
The vinyl acetate or. vinyl ether component is present in copolymer (B)
in an amount ranging from about 0 to about 30 percent by weight, the
(C2-12)alkyl(meth)acrylate component is present in said copolymer (B) in an
amount ranging from about 70 to about 98 percent by weight, the hydroxy
(C1.5)alkyl(meth)acrylate component is present in an amount ranging from
about 2 to about 20 percent by weight, and said polymerizable epoxy-
containing monomer is present in an amount ranging from about 0 to about 5
percent by weight.
It may be particularly desirable to avoid the use of vinyl acetate in a
composition which must meet ultra-clean standards to avoid the potential for
the production of an acid component upon hydrolysis of the vinyl acetate upon
contact with moisture in the ambient atmosphere.
Copolymers (A) and (B) are present in said composition in a weight
ratio ranging from about 0:100 to about 60:40, and preferably in a weight ratio
ranging from about 5:95 to about 40:60. The copolymers (A) and (B) may be
blended together by any suitable means such as mechanical mixing using a
propeller-type mixing blade.
Depending on the relative weight percentages of polymers (A) and (B),
and the compatibility of the blend, the final blend may have two separate Tg i values, or a single Tg value.
Copolymers (A) and (B) of the present invention can be prepared by any
suitable reaction technique such as free radical initiation techniques in the
presence of a solvent. Exemplary solvents include but are not limited to ethyl
acetate, cyclohexane, ketones or mixtures thereof. Solids content during
polymerization may typically range from about 40% to 60%. Exemplary free
radical initiators include but are not limited to peresters, acyl peroxides and
those of the azo type, such as 2,2'-azobis(isobutyronitrile)', benzoyl peroxide,
lauroyl peroxide, t-butyiperbenzoate, t-butyl peroxypivalate, dibenzyl
peroxydicarbonate, and diisopropyl peroxydicarbonate. Ultraviolet light and
ionizing radiation may also be employed. The free radical initiator is generally
present in the reaction mixture in an amount ranging from 0.01 to 10 % by wt.
based on the total weight of the monomers in the reaction mixture.
Typical polymerization temperatures range from 20 °C. to 150 °C. for
periods of time of from 2 to 24 hours until the desired degree of conversion
occurs. The resulting polymer will preferably exhibit a molecular weight in the
range of 50,000 to 2,000,000.
Various polymer compositions are known in the art which comprise a
glycidyl monomer and one or more of an acrylate and a nitrogen-containing
monomer.
U.S. Patent No. 6,200,639 discloses at column 8, lines 25-36 a
copolymer of glycidyl methacrylate and t-butyl methacrylate, optionally in
association with an aromatic vinyl-functional monomer, one or more hydroxyl-
fϊmctional (meth)acrylic monomers and one or more additional monomers.
U.S. Patent No. 5,723,191 discloses a tackified dual cure pressure
sensitive adhesive comprised of a copolymer having an acrylic backbone, a
glycidyl monomer, an unsaturated carboxylic acid monomer, and a vinyl
lactam monomer, together with a tackifier.
U.S. Patent No. 3,787,380 discloses a copolymer of N- vinyl orN-allyl
heterocyclic monomers, and unsaturated ester monomer and a glycidyl
monomer.
U.S. Patent Nos. 4,812,541 and 5,639,811 disclose a pressure sensitive
adhesive copolymer comprised of a N- vinyl lactam monomer, a glycidyl
monomer and an alkyl (meth) acrylate monomer.
U.S. Patent No. 5,270,416 discloses a thermosetting powder comprised
of a glycidyl monomer, a methyl (meth)acrylate, butyl acrylate and styrene.
U.S. Patent No. 3,857,905 discloses a thermosetting coating
composition comprised of a glycidyl monomer, a lower alkyl acrylate and a
methyl acrylate.
Various polymer compositions are also known in the art which are
comprised of both high and low Tg polymer components. See, for example,
U.S. Patent Nos. 3,846,368; 3,998,768; 4,107,235; 5,098,952; 5,098,956; and
5,827,609. U.S. Patent No. 5,827,609 discloses a multilayer pressure sensitive
adhesive construction where each layer exhibits a different glass transition
temperature.
Any conventional solvent/diluent may be admixed with the copolymer
blend to permit coating of the composition comprised of the blend of
copolymers (A) and (B) at a sufficiently low viscosity. Exemplary
solvents/diluents include but are not limited to xylene, toluene, butylacetate,
acetone, methyl ethyl ketone, methyl isobutyl ketone, alcohols such as
methanol, ethanol, propanol, butanol; ethylene glycol monomethyl ether,
ethylene glycol monobutyl ether acetate, ethylene glycol monoethyl ether
acetate, ethylene glycol monomethyl ether, ethylene glycol dibutyl ether;
hexane, mineral spirits, and other aliphatic, cycloaliphatic or aromatic
hydrocarbon solvents and other esters, ethers, ketones and alcohols, or mixtures
thereof.
The resulting blend may be coated onto a backing material by any
conventional manner, such as by roll coating, spray coating, or extrusion
coating, etc. by use of conventional extrusion devices. The blend may be
applied together with a solvent (typically having a solids content of about 30
percent by weight) and the solvent subsequently removed (such as by
evaporation) to leave the tacky adhesive layer on the backing material
(preferably having a solvent content of less than about 1 percent by weight).
Typically, evaporation will occur at a temperature in the range of from about
150 °F to about 250 °F to ensure removal of any solvent as well as to permit
crosslinking of the composition by thermocuring. Desirably, the coated
composition will have a thickness within the range of about 0.5 mil to about 50
mils.
Exemplary backing materials include but are not limited to flexible and
inflexible backing materials conventionally employed in connection with
pressure sensitive adhesives. Such materials include creped paper, kraft paper,
fabrics (knits, non-wovens, wovens), foil and synthetic polymer films or sheets
such as polyethylene, polypropylene, peel PMMA, polyvinyl chloride,
polyamide, polyimide, poly(ethylene terephthalate), polycarbonate, and
cellulose acetate, as well as glass, ceramics, metallized polymer films and other
composite sheet materials.
The adhesive may be applied to one or both of the aforementioned
backing materials, or sandwiched in alternating fashion between multiple layers
of the aforementioned backing materials, to yield two sided tapes. Also,
adhesives may be combined in discrete layers with or without benefit of a
backing material.
In another embodiment, the adhesive may be applied between two
release substrates or on a 2 side coated differential release substrate to form a
transfer adhesive.
Various additional components may also be incorporated into the
composition to modify the properties or characteristics thereof. A variety of
fillers may be incorporated into the polymer blend to provide desired physical
characteristics. For example, metallic flake filler such as stainless steel flake
having a particle size of 25-75 microns and aspect ratios of 31-94 may be
incorporated into the composition in an amount of up to about 60 percent by
weight to enhance vibration/sound-damping properties. Rigid polymers having
a high Tg such as polymethylmethacrylate may be added to produce a
controlled phase separation within the composition to further enhance
vibration/sound-damping of the composition. A variety of conventional
crosslinking compounds (such as blocked polyamines) may also be
incorporated into the composition to enhance crosslinking of the composition.
The present invention is illustrated by the following Examples which are
intended to be merely illustrative in nature and not limiting in scope.
EXAMPLE 1
A high Tg acrylic polymer (comprised of 40%» by wt. t-butyl
methacrylate, 10%> by wt. butyl acrylate, 20%> by wt. N-vinyl-2-pyrrolidone and
30% by wt. glycidyl methacrylate) was prepared in ethyl acetate solvent using
a free radical initiator l,l-di(t-amylperoxy)cyclohexane to a molecular weight
of approximately 200,000 GPC relative to polystyrene and having a first glass
transition temperature (Tg) of about 60°C (measured by DSC) and a second
glass transition temperature (Tg) of above 90°C.
5.76 parts of a low Tg acrylic polymer synthesized (25% by wt. solids in
ethyl acetate solvent) was mixed with 65.06 parts of a second copolymer
(comprised of about 70%> by wt. 2-ethylhexyl acrylate, about 20% by wt. vinyl
acetate, 10% by wt. hydroxyethylacrylate and 0.2% by wt. glycidyl
methacrylate, about 41% by wt. solids). 0.75 parts of Ancamine 2441 solution
in the mixture of isopropanol and methylethylketone solvents was used in the
formulation. The resulting adhesive was coated on polyester film and dried for
3 minutes at 90°C and 3 minutes at 140°C to yield films of various thicknesses.
Such films were colaminated to yield a thickness greater than 0.6 mm for
Dynamic Mechanical Analysis (DMA). The DMA Master Curve for frequency
ranging from 1 Hz to above 10 kHz was generated using a Rheometric
Scientific RAA Dynamic Mechanical Analyzer with a parallel plate fixture.
The Storage Modulus (G'), Loss Modulus (G") and the tan delta at different
frequency are summarized in Table 1 below:
Table 1
Dynamic mechanical analysis results
EXAMPLE 2
An adhesive blend comprised of 55.45 parts of a high Tg acrylic
polymer (synthesized from 40% by wt. t-butyl methacrylate, 10% by wt. butyl
acrylate, 20% by wt. N-vinyl-2-pyrrolidone and 30% by wt. glycidyl
methacrylate) and 137.08 parts of a low Tg acrylic polymer (41% by wt. solids
in ethyl acetate solvent of about 70% by wt. 2-ethylhexyl acrylate, about 20%
by wt. vinyl acetate, 10% by wt. hydroxyethylacrylate and 0.2% by wt.
glycidyl methacrylate) was prepared in the mixed solvent of ethyl acetate and
toluene. A 5-mil pressure sensitive adhesive film was generated by coating the
blend on polyester film and subsequently removing the solvent using the
following heating conditions: 5 minutes at 65.5°C, 5 minutes at 90°C and 5
minutes at 140°C. The DMA test results of Storage Modulus (G'), Loss
Modulus (G") and tan delta at 1 Hz, 100 Hz, 1 kHz and 10 kHz are summarized
in Table 2 below:
Table 2 Dynamic mechanical analysis results
The cleanliness of the pressure sensitive film was tested for leachable
ions using the ion chromatography analysis. An adhesive sample of 50 cm
placed on aluminum foil was rinsed with 18 Meg-Ohm water and submerged in
20 mis of 18 Meg-Ohm water for extraction at 85°C for one hour. Following
the extraction, the water was removed, filtered and tested for ionic cleanliness
using a Waters 636 Ion Chromatograph. As shown in Table 3 below, the
leachable ions are within the general acceptance criteria for Hard Disk Drive
industry, indicating the ultra high cleanliness of the adhesive composition.
Table 3
Summary of ionic chromatography test results
The same pressure sensitive adhesive sample was tested for outgassing
using Dynamic Headspace GC/MS and the test results are shown in Table 4
below:
Table 4
Summary of Outgassing test results
A high Tg acrylic polymer was synthesized in ethyl acetate solvent
based on the monomers of 2-ethyl hexyl acrylate (54% by wt.), hydroxy ethyl
acrylate (10% by wt.) and isobornyl methacrylate (36% by wt.), using free
radical initiators 2,2'-azobis-(2-methylbutyronitrile) (Vazo 67) and l,l'-azobis-
1-cyclohexanecarbonitrile (Vazo 88). 115.8 parts of the synthesized acrylic
polymer (about 53% solids in ethyl acetate) was blended with 223.1 parts of a
second acrylic polymer of low Tg (about 41% by wt. solids in ethyl acetate
solvent of about 70% by wt. 2-ethylhexyl acrylate, about 20% by wt. vinyl
acetate, 10% by. wt. hydroxyethylacrylate and 0.2% by wt. glycidyl
methacrylate). The resulting adhesive was coated on polyester film and dried
for 3 minutes at 90°C and 3 minutes at 140°C to generate films of various
thicknesses. Such films were colaminated to give thickness greater than 0.6
mm for Dynamic Mechanical Analysis (DMA). The DMA Master Curve for
frequency ranging from 1 Hz to above 10 kHz was generated using a
Rheometric Scientific RAA Dynamic Mechanical Analyzer with a parallel
plate fixture. The Storage Modulus (GO, Loss Modulus (G") and tan delta at
different frequency were shown in Table 5 below:
Table 5
Dynamic mechanical analysis results