U.S. patent application number 12/334904 was filed with the patent office on 2010-06-17 for non-woven sheet containing fibers with sheath/core construction.
This patent application is currently assigned to E. I. DU PONT DE NEMOURS AND COMPANY. Invention is credited to DAVID MATTHEWS LAURA, JR., XUN MA, PAUL ELLIS ROLLIN, JR..
Application Number | 20100151760 12/334904 |
Document ID | / |
Family ID | 41818691 |
Filed Date | 2010-06-17 |
United States Patent
Application |
20100151760 |
Kind Code |
A1 |
LAURA, JR.; DAVID MATTHEWS ;
et al. |
June 17, 2010 |
NON-WOVEN SHEET CONTAINING FIBERS WITH SHEATH/CORE CONSTRUCTION
Abstract
A non-woven sheet contains sheath/core polymer fibers with the
polymer in the sheath having a melting point at least 15 degrees
centigrade higher than the melting point of the polymer of the
core. The fibers have an average diameter greater than 7 microns
and the sheet has a normalized air resistance greater than
0.25/(g/m.sup.2).
Inventors: |
LAURA, JR.; DAVID MATTHEWS;
(MIDLOTHIAN, VA) ; MA; XUN; (MIDLOTHIAN, VA)
; ROLLIN, JR.; PAUL ELLIS; (HENDERSONVILLE, TN) |
Correspondence
Address: |
E I DU PONT DE NEMOURS AND COMPANY;LEGAL PATENT RECORDS CENTER
BARLEY MILL PLAZA 25/1122B, 4417 LANCASTER PIKE
WILMINGTON
DE
19805
US
|
Assignee: |
E. I. DU PONT DE NEMOURS AND
COMPANY
|
Family ID: |
41818691 |
Appl. No.: |
12/334904 |
Filed: |
December 15, 2008 |
Current U.S.
Class: |
442/364 ;
264/172.15; 442/361 |
Current CPC
Class: |
B32B 2262/0261 20130101;
B32B 2262/0276 20130101; B32B 7/02 20130101; B32B 2457/00 20130101;
B32B 2307/206 20130101; B32B 2307/702 20130101; B32B 5/022
20130101; B32B 2307/5825 20130101; B32B 2262/14 20130101; B32B
27/40 20130101; B32B 7/12 20130101; B32B 5/08 20130101; B32B 27/12
20130101; B32B 27/36 20130101; B32B 2262/0284 20130101; Y10T
442/637 20150401; B32B 27/18 20130101; D04H 3/16 20130101; B32B
2307/718 20130101; D04H 3/14 20130101; B32B 2262/0253 20130101;
B32B 27/32 20130101; B32B 2262/12 20130101; Y10T 442/641 20150401;
B32B 2307/7242 20130101 |
Class at
Publication: |
442/364 ;
442/361; 264/172.15 |
International
Class: |
D04H 3/16 20060101
D04H003/16; D01D 5/28 20060101 D01D005/28 |
Claims
1. A non-woven sheet comprising: a network of
substantially-continuous thermoplastic polymer filaments, the
polymer filaments each individually comprising a plurality of
polymers including at least a first polymer and a second polymer,
the melting point of the first polymer being at least 15 degrees C.
higher than the melting point of the second polymer, the individual
polymer filaments further characterized in that (1) the first
polymer comprises from 10 to 70 weight percent of the total weight
of the first and second polymer, (2) the second polymer comprises
from 30 to 90 weight percent of the total weight of the first and
second polymer and, the network of filaments being consolidated and
fused such that (a) the first polymer forms a continuous phase in
the fused consolidated network and (b) the second polymer forms a
disperse phase in the fused consolidated network wherein the
consolidated network has a porosity such that the normalized air
resistance of the network is at least 0.2 s/(g/m.sup.2).
2. The non-woven sheet of claim 1 wherein the first polymer is
selected from the group comprising polyarylene sulfide, polyimide,
liquid crystalline polyester, fluoropolymer and mixtures
thereof.
3. The non-woven sheet of claim 2 wherein the polyarylene sulfide
is polyphenylene sulfide.
4. The non-woven sheet of claim 1 wherein the second polymer is
selected from the group comprising polyolefin, polyester, polyamide
and mixtures thereof.
5. The non-woven sheet of claim 2 wherein the polyester is
polyethylene terephthalate.
6. An electrical insulation component for an electrical device
comprising the non-woven sheet of claim 1.
7. Insulation useful for an electrical device comprising a
polymeric film positioned adjacent to, and attached to, one or more
non-woven sheets said non-woven sheets comprising: a network of
substantially-continuous thermoplastic polymer filaments, the
polymer filaments each individually comprising a plurality of
polymers including at least a first polymer and a second polymer,
the melting point of the first polymer being at least 15 degrees C.
higher than the melting point of the second polymer, the individual
polymer filaments further characterized in that (1) the first
polymer comprises from 10 to 70 weight percent of the total weight
of the first and second polymer, (2) the second polymer comprises
from 30 to 90 weight percent of the total weight of the first and
second polymer and, the network of filaments being consolidated and
fused such that (a) the first polymer forms a continuous phase in
the fused consolidated network and (b) the second polymer forms a
disperse phase in the fused consolidated network wherein the
consolidated network has a porosity such that the normalized air
resistance of the network is greater than 0.2 s/(g/m.sup.2).
8. The insulation of claim 7 wherein, the polymeric film is a
polyester film.
9. The insulation of claim 7 having the form of a slot liner, a
closure, a wedge or a stick.
10. An electrical device comprising the insulation of claim 7.
11. A method for producing a non-woven sheet of multicomponent
polymeric fiber comprising the steps of: (i) melt spinning at
between 3500 to 5000 m/min in the presence of an attenuating force
provided by a rectangular slot jet a fiber having an average fiber
diameter greater than 7 microns, said fiber further comprising an
amorphous sheath component of from 10 to 70 weight percent of a
first polymer based on the total weight of polymer in the core and
sheath and a core component of from 30 to 90 weight percent of a
fibrous second polymer based on the total weight of polymer in the
core and sheath, wherein the melting point of the first polymer is
at least 15 degrees C. higher than the melting point of the second
polymer, (ii) forming a non-woven web of fibers on a forming belt,
(iii) passing the non-woven web of fibers through heated bonding
rolls to fuse the fibers and thereafter, (iv) smooth calendering
said fused fiber web to convert the amorphous sheath of first
polymer material into a substantially crystalline continuous phase
and further compact and density the non-woven web to embed the
fibrous second polymer into the continuous phase of the first
polymer and to achieve a web having a normalized air resistance
greater than 0.2 s/(g/m.sup.2).
12. The method of claim 11 wherein the first polymer is selected
from the group comprising polyarylene sulfide, polyimide, liquid
crystalline polyester, fluoropolymer and mixtures thereof.
13. The method of claim 12 wherein the polyarylene sulfide is
polyphenylene sulfide.
14. The method of claim 11 wherein the second polymer is selected
from the group comprising polyolefin, polyester, polyamide and
mixtures thereof.
15. The non-woven sheet of claim 14 wherein the polyester is
polyethylene terephthalate.
Description
BACKGROUND OF INVENTION
[0001] 1. Field of the Invention
[0002] The present invention is directed to a non-woven sheet
having improved characteristics due to the selection of specific
fibers.
[0003] 2. Description of Related Art
[0004] U.S. Patent Application Publication No. 2005/0269011 A1
discloses a method for making a spunbonded fabric from a blend of
polyarylene sulfide and a crystal enhancer. U.S. Pat. No. 6,949,288
discloses a multicomponent fiber with a polyarylene sulfide
component and incorporation of the fibers into various
products.
[0005] There is a need for a non-woven sheet having superior
properties to known fabrics.
SUMMARY OF INVENTION
[0006] The present invention is directed to a non-woven sheet
comprising multicomponent polymeric fibers having an average fiber
diameter greater than 7 microns, said fibers further
comprising:
[0007] (a) a sheath component of from 10 to 70 weight percent of a
first polymer based on the total weight of polymer in the core and
sheath (b) a core component of from 30 to 90 weight percent of a
second polymer based on the total weight of polymer in the core and
sheath, wherein the melting point of the first polymer is at least
15 degrees C. higher than the melting point of the second
polymer,
[0008] the non-woven sheet being further characterized by having a
normalized air resistance greater than 0.2 s/(g/m.sup.2).
[0009] The non-woven sheet particularly in combination with a
further dielectric sheet is useful as an insulating material.
BRIEF DESCRIPTION OF FIGURES
[0010] FIG. 1 depicts a typical process for making fiber and
forming the fibers into a non-woven web or sheet.
[0011] FIG. 2 shows the additional calendaring process utilized in
this invention.
DETAILED DESCRIPTION OF THE INVENTION
Definitions:
[0012] By multicomponent fibers it is meant the fiber is comprised
of more than one polymer. In one preferred embodiment the fiber is
bicomponent, meaning it is melt spun with two thermoplastic
polymers in a sheath-core arrangement.
[0013] The phrase "more than one polymer" is meant to include not
only polymers having different chemical structures, but polymers
having similar structures but having different melting points.
[0014] By nonwoven it is meant an assembly of textile fibers in a
random web or mat held together by mechanical interlocking, by
fusing of the fibers or by bonding with a cementing medium.
Discussion:
[0015] A preferred final article of the present invention is a
non-woven sheet having a normalized air resistance greater than
0.25/(g/m.sup.2) in combination with a dielectric film with the
article suitable for use in electrical insulation. The non-woven
sheet has superior mechanical strength, initial tear resistance and
elongation.
[0016] The non-woven sheet is made from multicomponent sheath/core
polymeric fibers having an average diameter greater than 7 microns.
A preferred range of average fiber diameter is in a range from 14
to 21 microns.
[0017] For purposes of illustration, the multicomponent sheath/core
polymeric fibers can be round, trilobal, pentalobal, octalobal,
like a Christmas tree, dumbbell-shaped, island-in-the-sea or
otherwise star shaped in cross section. The fibers may also be in a
side by side arrangement. The polymer component of the sheath is
referred to as the first polymer and the polymer component of the
core is referred to as the second polymer
[0018] The core component contains a second polymer present in a
range from 30 to 90 weight percent based on the total weight of
polymer in the core and sheath. Accordingly, the sheath component
contains a first polymer in a range from 10 to 70 weight percent. A
preferred range for the second polymer is in a range from 30 to 50
weight percent and accordingly a preferred range for the first
polymer is in a range from 50 to 70 weight percent.
[0019] A further requirement in the sheath/core construction of the
fibers is the melting point of the first polymer (the sheath) which
is at least 15 degrees centigrade higher than the melting point of
the second polymer (the core). Typically, the difference in melting
points is at least 20 degrees centigrade. Accordingly, the sheath
has a higher thermal stability than the core.
[0020] One preferred embodiment of the present invention is
directed to a non-woven sheet made from sheath/core fibers wherein
the core is formed from polymers such as polyolefin, polyester or
polyamide (the second polymer) and the sheath is formed from melt
processable polymers such as polyarylene sulfide, polyimide, liquid
crystalline polyester or polytetrafluoroethylene (the first
polymer). In a preferred embodiment, the sheath contains
polyphenylene sulfide having an estimated zero shear viscosity of
from 2300 to 2700 Poise when measured at 300.degree. C. and the
core component is polyethyleneterephthalate.
[0021] The first and second polymers either alone or in combination
may include polyolefin, polyester or polyamide in the second
polymer and polyarylene sulfide, polyimide, liquid crystalline
polyester or polytetrafluoroethylene in the first polymer provided
the melting point of the sheath is at least 15.degree. C. higher
than the melting point of the core.
[0022] The polymeric components forming the multicomponent fibers
can include conventional additives such as dyes, pigments,
antioxidants, ultraviolet stabilizers, spin finishes, and the like.
The use of crystallinity enhancing additives in the polymeric
compositions is optional.
[0023] Prior art processes that form a non-woven sheet having
multicomponent fibers can be used, including processes that form
the sheet solely from multicomponent fibers in staple form. Such
staple fiber non-wovens can be prepared by a number of methods
known in the art, including carding or garneting, air-laying, or
wet-laying of fibers. The staple fibers preferably have a denier
per filament between about 0.5 and 6.0 and a fiber length of
between about 0.6 cm and 10 cm.
[0024] The fibers in the non-woven sheet can be continuous
filaments directly spun into the sheet without any intentional
cutting of the filaments. The non-woven sheet can be made from
processes as outlined in FIG. 1 to spin and consolidate continuous
filament thermoplastic webs known in the art as spunbonding or
meltblowing. An attenuating force should be provided to the bundle
of fibers by a rectangular slot jet. By spinning the fiber at line
speeds from 3500 to 5000 m/min, a significant amount of the second
polymer is crystallized while the first polymer is not. Multiple
component spunbonded webs suitable for preparing laminate parts can
be prepared using methods known in the art, for example as
described in U.S. Pat. No 6,548,431 to Bansal et al. Multicomponent
fibers can be incorporated into a non-woven sheet by melt spinning
fibers from spinning beams having a large number of holes onto a
moving horizontal belt as disclosed in U.S. Pat. No. 5,885,909 to
Rudisill et al. Continuous filament webs suitable for preparing the
non-woven fabrics preferably comprise continuous filaments having a
denier per filament between 0.5 and 20 with a preferred denier per
filament range of 1 and 5.
[0025] The non-woven sheet must be subjected to a further
calendering step as shown in FIG. 2 to give a sheet having the
desired level of porosity, degree of crystallinity of the first
polymer and basis weight. This calendaring step may be carried out
as a separate operation or integrated into the web forming line of
FIG. 1 and located after the filament bonding rolls. During the
calendering process, the sheath polymer, which is substantially
amorphous, flows, becomes substantially crystalline and forms a
continuous phase. A measure of the extent of the continuous phase
is sheet porosity or air permeability with a highly continuous
phase having a low air permeability. Some increase in crystallinity
of the core material is also observed. The core fibers, however,
remain as discrete domains of fibrous filaments in a continuous
phase of sheath material. Parameters necessary to give good
calendered non-woven sheet properties such as roll temperature,
roll pressure, line speed and contact time with the rollers vary
depending on the polymeric composition of the fiber sheath and, to
a lesser extent, to the polymeric composition of the core.
Calendering can be carried out in the temperature range of from
90.degree. C. to 240.degree. C. with higher temperatures permitting
faster line speeds. Preferable calendering conditions are about
200.degree. C. at a nip pressure of about 3500 N/cm. This produces
a non-woven sheet or web having a porosity, as measured by
normalized air resistance, of at least 0.2 s/gsm and a basis weight
in the range from 30 to 350 gsm. More preferably, normalized air
resistance is in the range of from 0.2 to 5.0 s/gsm. More
preferably, the basis weight range is from 30-300 gsm and most
preferably from 50-150 gsm. The calendering process did not cause
any deterioration in the tear strength of the calendered non-woven
sheet when compared to the tear strength of a non-calendered sheet
made in accordance with FIG. 1.
[0026] The non-woven sheet can be used with a film to make a
composite laminate suitable for use in electrical insulation. In
such a laminate, the film provides the desired dielectric
properties and the low porosity non-woven sheet minimizes loss of
those dielectric properties. The film is positioned adjacent to,
and attached to at least one non-woven sheet to form the composite.
Where two non-woven sheets are used, the film is sandwiched between
the two sheets which allow the composite laminate to be impregnated
with a matrix resin or varnish either prior to installation in an
electrical device, or after installation in the device. The
impregnation resin may also include additives. The film is attached
to the non-woven sheets by an adhesive which may be a film, liquid,
powder or paste. The cure temperature of the adhesive must be lower
than the melting point of the polymers of the fiber, preferably by
at least ten degrees centigrade. Either a thermoset or
thermoplastic adhesive may be used. A urethane adhesive is
particularly suitable. In some circumstances, if a PPS film or a
bondable film is employed, thermal lamination may also be possible.
Suitable bondable films include PET films that have an amorphous
PET layer or layers on the outside of a PET film. Suitable PPS
films for thermal lamination include Torelina.RTM. PPS from
Toray.
[0027] While a single layer non-woven sheet on either side of the
film is a preferred embodiment, a multi-layer non-woven could be
used as long as the layer of the multi-layer non-woven that is in
contact with the film is made from the multicomponent fibers as
previously described. Basis weight and thickness of the non-woven
sheet is not critical and is dependent upon the end use of the
final laminate. In some preferred embodiments the basis weight is
50 to 150 grams per square meter and the final thickness of the
non-woven sheets in the laminate structure is 50 to 125
micrometers.
[0028] Any suitable film can be used. If a thermoplastic film is
selected, useful examples include polyester, polyamide,
poly(phenylene sulfide) (PPS), and/or other thermoplastic
materials. The thermoplastic film can be a homogeneous material or
it can be layered structure with different thermoplastics in
different layers. In some embodiments, the preferred polyesters
include poly(ethylene terephthalate), poly(ethylene naphthalate),
and liquid crystalline polyesters.
[0029] Poly(ethylene terephthalate) (PET) can include a variety of
comonomers, including diethylene glycol, cyclohexanedimethanol,
poly(ethylene glycol), glutaric acid, azelaic acid, sebacic acid,
isophthalic acid, and the like. In addition to these comonomers,
branching agents like trimesic acid, pyromellitic acid,
trimethylolpropane and trimethyloloethane, and pentaerythritol may
be used. The poly(ethylene terephthalate) can be obtained by known
polymerization techniques from either terephthalic acid or its
lower alkyl esters (e.g. dimethyl terephthalate) and ethylene
glycol or blends or mixtures of these. Poly(ethylene napthalate)
(PEN) can be obtained by known polymerization techniques from 2,6
napthalene dicarboxylic acid and ethylene glycol. Examples of
commercially available PET and PEN films are MYLAR.RTM. and
TEONEX.RTM. films respectively, sold by DuPont-Teijin Films.
[0030] By "liquid crystalline polyester" (LCP) herein is meant
polyester that is anisotropic when tested using the TOT test or any
reasonable variation thereof, as described in U.S. Pat. No.
4,118,372. One preferred form of liquid crystalline polyesters is
fully aromatic. Possible LCP compositions for films and film types
are described, for example, in U.S. Pat. No. 5,248,530 to Jester et
al. One commercially available example of PPS film is TORELINA.RTM.
film sold by Toray Company.
[0031] Other materials, particularly those often found in or made
for use in thermoplastic compositions may also be present in the
film. These materials should preferably be chemically inert and
reasonably thermally stable under the operating environment of the
part in service. Such materials may include, for example, one or
more of fillers, reinforcing agents, dyes, pigments, antioxidants,
stabilizers and nucleating agents. Other polymers may also be
present, thus forming polymer blends. In some embodiments, the
composition can contain about 1 to about 55 weight percent of
fillers and/or reinforcing agents, more preferably about 5 to about
40 weight percent of these materials.
[0032] In one embodiment the thermoplastic film can also contain an
internal layer of thermoset material. For example, KAPTON.RTM. EKJ
film, sold by DuPont, has thermoplastic polyimide outside layers
with a thermoset polyimide layer inside the structure.
[0033] Thermal lamination processes to make the composite are well
known in the art and include batch processes such as a platen press
or vacuum bag or a continuous process such as a double belt
press.
[0034] In the following examples all parts and percentages are by
weight and degrees in centigrade unless otherwise indicated.
Test Methods
[0035] Tensile strength and elongation to break of the non-woven
sheets were measured on an Instron-type testing machine using test
specimens 2.54 cm wide and a gage length of 18 cm, in accordance
with ASTM D 828-97. Only the machine direction results are
reported.
[0036] Initial tear resistance was also measured on an Instron-type
testing machine in accordance with ASTM D 1004-07 with a gauge
length of 7.62 cm. Only the machine direction results are
reported.
[0037] The thickness of non-woven sheets was measured in accordance
with ASTM D374-99 Method E. The basis weight of the non-woven
sheets was taken according to ASTM D 646-96.
[0038] The air resistances of the non-woven sheets were measured in
accordance with TAPPI T 460 om-02 as the amount of time to pass 100
ml of air through the sheets at a pressure differential of 1.22
kPA. The data is reported in seconds.
[0039] Normalized air resistance was calculated by dividing the air
resistance in seconds (determined by TAPPI 460 om-02) by the basis
weight in grams per square meter (determined by ASTM D 646-96). In
some instances as noted in Table 2, the air resistance measured
according to TAPPI T 460 was below the recommended minimum of 5
seconds. For these samples, the time to pass 300 ml of air through
the sheets at a pressure differential of 1.22 kPA was taken. This
time was divided by a factor of 3 in order to provide a basis of
comparison of samples that complied with the recommended minimum
time of 5 seconds for 100 ml of air with those that required a
larger volume of air to obtain a meaningful result. Also where
noted, the air resistance of the sheet was too low to be measured
using either 100 ml or 300 ml of air. In these cases, the air
resistance is assumed to be near zero.
[0040] Melting points and enthalpies of fusion and crystallization
were measured by ASTM Method D3418. Melting points are taken as the
maximum of the melting endotherm and are measured on the first
heating cycle using a Differential Scanning Calorimeter (DSC) at a
heating rate of 10.degree. C./min.
[0041] Average fiber diameter was determined as follows. A bundle
of fibers was carefully collected just below the attenuating jet.
The fiber bundle was then prepared for viewing under an optical
microscope. A digital image of the fiber bundle was then captured
with the aid of computer. The diameter of at least thirty (30)
clearly distinguishable fine fibers were measured from the
photographs and recorded. Defects were not included (i.e., lumps of
fine fibers, polymer drops, intersections of fine fibers). The
average (mean) fiber diameter for each sample was calculated.
[0042] X-ray diffraction samples were run on a PANalytical X'Pert
MPD diffractometer using copper radiation. The analysis was run in
reflection mode using fixed 1/2 deg. slits for the incident and
diffracted beam optics and a 0.3 mm receiving slit. This unit had a
proportional detector with a curved graphite monochromator. Scan
parameters were 5-40 degrees two-theta with a step size of 0.15
degree at 20 seconds per point. The instrument was calibrated using
a sample of silicon provided by PANalytical.
[0043] Scanning Electron Microscope (SEM) imaging samples were cut
from the appropriate examples and placed on aluminum SEM stubs. The
stubs were placed in a sputter coater and coated for 80-100 seconds
with a thin layer (1-2 angstroms) of gold/palladium. This coating
serves as the necessary conductor for the SEM. The stubs were
inserted in a mount and placed in the SEM chamber. After pumping
down to vacuum, each sample is imaged at different magnifications,
at working distances of 8-11 mm in secondary emission (SE) mode.
All images were captured and saved electronically. Some examples
were soaked in hexaflouro isoproponol (HFIP) at room temperature
for 3-4 hours to dissolve out the PET from the PET/PPS matrix.
Samples of these examples were cut in to 2''.times.6'' strips and
immersed in 100 ml of HFIP for 3-4 hours. After soaking, the
samples were removed from the HFIP solution, rinsed with methanol
and allowed to air dry.
EXAMPLE 1
[0044] In this example, a bicomponent spunbond fabric was made from
a poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E. I. duPont de
Nemours, Wilmington, Del. under the tradename Crystar.RTM.
polyester (Merge 4415). The PPS component, available from Ticona
Engineering Polymers, Florence, Ky. under the tradename
Fortron.RTM. PPS was a mixture of 70 wt % grade 0309 C1 and 30 wt %
grade 0317 C1. The PPS component had an estimated zero shear
viscosity of approximately 2500 Poise measured at 300.degree. C.
The PET resin was dried in a through air dryer at a temperature of
120.degree. C. to a moisture content of less than 50 parts per
million. The PPS resins were dried in a through air dryer at a
temperature of 115.degree. C. to a moisture content of less than
150 parts per million. The PET polymers were heated in an extruder
at 290.degree. C. and the PPS resins heated in a separate extruder
at 295.degree. C. The two polymers were metered to a spin-pack
assembly where the two melt streams were separately filtered and
then combined through a stack of distribution plates to provide
multiple rows of spunbond fibers having sheath-core cross sections.
Such processing is well known to those skilled in the art. The PET
component comprised the core and the PPS component comprised the
sheath.
[0045] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 0.8
g/hole/min. The PET component consisted of 70% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 50.1 m/min. A vacuum was applied underneath the
belt to help pin the fibers to the belt. The fibers had an average
diameter of 14.5 microns. The spunbond layer was then passed
between an embosser roll and an anvil roll as shown in FIG. 1 to
achieve filament to filament bonding. The bonding conditions were
135.degree. C. roll temperature and 875 N/cm nip pressure. After
thermal bonding, the spunbond sheet was formed into a roll using a
winder.
[0046] In an additional step, the non-woven web was then
smooth-calendered to achieve further densification of the already
bonded non-woven web. The process used is shown in FIG. 2. Line
speed was 18.3 m/min. Calender rolls 1 and 4 were smooth unheated
rolls with a nylon composite shell having an outside diameter of 50
cm. Calender rolls 2 and 3 were heated stainless steel rolls having
an outside diameter of 46 cm. The steel rolls were heated to a
surface temperature of 200.degree. C. The sheet was passed through
a nip between calender rolls 1 and 2 under a nip pressure of 3100
N/cm. The sheet then traveled around Calender roll 2 and passed
through the open nip between calender rolls 2 and 3. The sheet then
wrapped around Calender roll 3 and through the nip between calender
rolls 3 and 4. The nip pressure between calender rolls 3 and 4 was
3500 N/cm. After calendering, the spunbond sheet had a basis weight
of 90 g/m.sup.2.
EXAMPLE 2
[0047] In this example, a bicomponent spunbond fabric was made from
a poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E. I. duPont de
Nemours under the tradename Crystar.RTM. polyester (Merge 4415).
The PPS component, available from Ticona Engineering Polymers under
the tradename Fortron.RTM. PPS was a mixture of 70 wt % grade 0309
C1 and 30 wt % grade 0317 C1. The PPS component had an estimated
zero shear viscosity of approximately 2500 Poise measured at
300.degree. C. The PET resin was dried in a through air dryer at a
temperature of 120.degree. C. to a moisture content of less than 50
parts per million. The PPS resins were dried in a through air dryer
at a temperature of 115.degree. C. to a moisture content of less
than 150 parts per million. The PET polymers were heated in an
extruder at 290.degree. C. and the PPS resins heated in a separate
extruder at 295.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the PPS
component comprised the sheath.
[0048] A spin pack assembly consisting of 2158 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 1.4
g/hole/min. The PET component consisted of 50% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 43.8 m/min. The fibers had an average diameter of
17.5 microns. A vacuum was applied underneath the belt to help pin
the fibers to the belt. The spunbond layer was then passed between
an embosser roll and an anvil roll as shown in FIG. 1 to achieve
filament to filament bonding. The bonding conditions were
135.degree. C. roll temperature and 875 N/cm nip pressure. After
thermal bonding, the spunbond sheet was formed into a roll using a
winder.
[0049] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 78
g/m.sup.2.
[0050] An etched cross sectional view of this non woven web was
examined under a scanning electron microscope. The etching medium
was hexafluoroisopropanol (HFIP) which dissolved the polyester
component but left the PPS material intact. The continuous
crystalline phase of PPS could be clearly seen as well as voids
where the PET fibrous component was removed.
EXAMPLE 3
[0051] In this example, a bicomponent spunbond fabric was made from
a poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E. I. duPont de
Nemours under the tradename Crystar.RTM. polyester (Merge 4415).
The PPS component, available from Ticona Engineering Polymers under
the tradename Fortron.RTM. PPS was a mixture of 70 wt % grade 0309
C1 and 30 wt % grade 0317 C1. The PPS component had an estimated
zero shear viscosity of approximately 2500 Poise measured at
300.degree. C. The PET resin was dried in a through air dryer at a
temperature of 120.degree. C. to a moisture content of less than 50
parts per million. The PPS resins were dried in a through air dryer
at a temperature of 115.degree. C. to a moisture content of less
than 150 parts per million. The PET polymers were heated in an
extruder at 290.degree. C. and the PPS resins heated in a separate
extruder at 295.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the PPS
component comprised the sheath.
[0052] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 1.0
g/hole/min. The PET component consisted of 60% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 65.9 m/min. A vacuum was applied underneath the
belt to help pin the fibers to the belt. The spunbond layer was
then passed between an embosser roll and an anvil roll as shown in
FIG. 1 to achieve filament to filament bonding. The bonding
conditions were 135.degree. C. roll temperature and 1050 N/cm nip
pressure. After thermal bonding, the spunbond sheet was formed into
a roll using a winder.
[0053] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 76
g/m.sup.2.
EXAMPLE 4
[0054] In this example, a bicomponent spunbond fabric was made from
poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.67 dl/g and is available from E. I. DuPont de
Nemours under the tradename Crystar.RTM. polyester (Merge 4434).
The PPS component, available from Ticona Engineering Polymers under
the tradename Fortron.RTM. PPS, was a mixture of 70 wt % grade 0309
C1 and 30 wt % grade 0317 C1. The PPS component had an estimated
zero shear viscosity of approximately 2500 Poise measured at
300.degree. C. The PET resin was dried in a through air dryer at a
temperature of 120.degree. C. to a moisture content of less than 50
parts per million. The PPS resins were dried in a through air dryer
at a temperature of 115.degree. C. to a moisture content of less
than 150 parts per million. The PET polymers were heated in an
extruder at 290.degree. C. and the PPS resins heated in a separate
extruder at 295.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the PPS
component comprised the sheath.
[0055] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 0.8
g/hole/min. The PET component consisted of 70% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 52.7 m/min. A vacuum was applied underneath the
belt to help pin the fibers to the belt. The spunbond layer was
then passed between an embosser roll and an anvil roll as shown in
FIG. 1 to achieve filament to filament bonding. The bonding
conditions were 135.degree. C. roll temperature and 1050 N/cm nip
pressure. After thermal bonding, the spunbond sheet was formed into
a roll using a winder.
[0056] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 78
g/m.sup.2.
EXAMPLE 5
[0057] In this example, a bicomponent spunbond fabric was made from
poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E.I. DuPont de Nemours
under the tradename Crystar.RTM. polyester (Merge 4415). The PPS
component had a melt flow index of 101 g/10 min at 316.degree. C.
under a load of 2.16 kg and is available from Ticona Engineering
Polymers under the tradename Fortron PPS 0309 C1. The PET resin was
dried in a through air dryer at a temperature of 120.degree. C. to
a moisture content of less than 50 parts per million. The PPS
resins were dried in a through air dryer at a temperature of
115.degree. C. to a moisture content of less than 150 parts per
million. The PET polymers were heated in an extruder at 290.degree.
C. and the PPS resins heated in a separate extruder at 295.degree.
C. The two polymers were metered to a spin-pack assembly where the
two melt streams were separately filtered and then combined through
a stack of distribution plates to provide multiple rows of spunbond
fibers having sheath-core cross sections. The PET component
comprised the core and the PPS component comprised the sheath.
[0058] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 0.8
g/hole/min. The PET component consisted of 50% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 50.1. The fibers had an average diameter of 14.5
microns. A vacuum was applied underneath the belt to help pin the
fibers to the belt. The spunbond layer was then passed between an
embosser roll and an anvil roll as shown in FIG. 1 to achieve
filament to filament bonding. The bonding conditions were
120.degree. C. roll temperature and 350 N/cm nip pressure. After
thermal bonding, the spunbond sheet was formed into a roll using a
winder.
[0059] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 83
g/m.sup.2.
EXAMPLE 6
[0060] In this example, a bicomponent spunbond fabric was made from
poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E. I. DuPont de
Nemours under the tradename Crystar.RTM. polyester (Merge 4415).
The PPS component, available from Ticona Engineering Polymers under
the tradename Fortron.RTM. PPS, was a mixture of 70 wt % grade 0309
C1 and 30 wt % grade 0317 C1. The PPS component had an estimated
zero shear viscosity of approximately 2500 Poise measured at
300.degree. C. The PET resin was dried in a through air dryer at a
temperature of 120.degree. C. to a moisture content of less than 50
parts per million. The PPS resins were dried in a through air dryer
at a temperature of 115.degree. C. to a moisture content of less
than 150 parts per million. The PET polymers were heated in an
extruder at 290.degree. C. and the PPS resins heated in a separate
extruder at 295.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the PPS
component comprised the sheath.
[0061] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 1.0
g/hole/min. The PET component consisted of 50% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 83.4 m/min. A vacuum was applied underneath the
belt to help pin the fibers to the belt. The spunbond layer was
then passed between an embosser roll and an anvil roll as shown in
FIG. 1 to achieve filament to filament bonding. The bonding
conditions were 135.degree. C. roll temperature and 875 N/cm nip
pressure. After thermal bonding, the spunbond sheet was formed into
a roll using a winder.
[0062] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 53
g/m.sup.2.
EXAMPLE 7
[0063] In this example, a bicomponent spunbond fabric was made from
poly(ethylene terephthalate) (PET) component and a poly(phenylene
sulfide) (PPS) component. The PET component had an intrinsic
viscosity of 0.63 dl/g and is available from E. I. DuPont de
Nemours under the tradename Crystar.RTM. polyester (Merge 4415).
The PPS component, available from Ticona Engineering Polymers under
the tradename Fortron.RTM. PPS, was a mixture of 70 wt % grade 0309
C1 and 30 wt % grade 0317 C1. The PPS component has an estimated
zero shear viscosity of approximately 2500 Poise measured at
300.degree. C. The PET resin was dried in a through air dryer at a
temperature of 120.degree. C. to a moisture content of less than 50
parts per million. The PPS resins were dried in a through air dryer
at a temperature of 115.degree. C. to a moisture content of less
than 150 parts per million. The PET polymers were heated in an
extruder at 290.degree. C. and the PPS resins heated in a separate
extruder at 295.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the PPS
component comprised the sheath.
[0064] A spin pack assembly consisting of 4316 round capillary
openings was heated to 295.degree. C. and the PPS and PET polymers
spun through each capillary at a polymer throughput rate of 1.0
g/hole/min. The PET component consisted of 50% by weight of the
total weight of the spun bond fibers. The fibers were cooled in a
cross flow quench extending over a length of 122 cm. An attenuating
force was provided to the bundle of fibers by a rectangular slot
jet. The distance between the spin-pack to the entrance of the jet
was 92.5 cm. The fibers exiting the jet were collected on a forming
belt traveling at 71.5 m/min. A vacuum was applied underneath the
belt to help pin the fibers to the belt. The spunbond layer was
then passed between an embosser roll and an anvil roll as shown in
FIG. 1 to achieve filament to filament bonding. The bonding
conditions were 145.degree. C. roll temperature and 875 N/cm nip
pressure. After thermal bonding, the spunbond sheet was formed into
a roll using a winder. A DSC spectrum of this non-woven web
material had an exothermic peak or cold crystallization peak of
11.63 J/g at 119.degree. C. associated with the enthalpy of
crystallization of one or both components, and endothermic peaks of
24.08 J/g at 258.degree. C. and 12.37 J/g at 281.degree. C.,
associated with the melting points of the PET and the PPS
components respectively. A wide angle X-ray diffraction pattern was
taken of this spunbond sheet and showed no evidence of PPS
crystallinity in the spectrum. Some PET crystallinity was
evident.
[0065] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 68
g/m.sup.2. A DSC spectrum of the material after this smooth
calendering step had no exothermic peak at 119.degree. C. but the
endothermic peaks at 258.degree. C. and 281.degree. C., associated
with the enthalpy of fusion of the PET and PPS components remained.
Based on the mass of PPS, which comprised 50 wt % of this example,
the difference in magnitude between the enthalpy of crystallization
before calendering and the PPS enthalpy of fusion after calendering
was 1.42 J/g. The difference between the two DSC spectra of Example
7 indicates that the additional smooth calendering process step
significantly increases the degree of crystallinity of the
components of the fiber. They are now substantially crystalline. A
wide angle X-ray diffraction pattern was taken of the calendered
spunbond sheet and showed peaks associated with PPS crystallinity.
In addition the peaks associated with PET crystallinity increased
in intensity. This again confirms that the calendering step
converts amorphous PPS into a crystalline phase and further
enhances PET crystallinity. The reference document for identifying
crystalline PPS in both the uncalendered and calendered sheets is
"X-Ray Diffraction Analysis Technique for Determining the Polymer
Crystallinity in a Polyphenylene Sulfide Composite by Lee et al,
Polymer Composites, December 1995, Vol 16, No 6, pages 481 to
488.
COMPARATIVE EXAMPLE A
[0066] In this example, a single component spunbond fabric was made
from poly(phenylene sulfide) (PPS). The PPS had a melt flow index
of 101 g/10 min at 316.degree. C. under a load of 2.16 kg and is
available from Ticona Engineering Polymers under the tradename
Fortron PPS 0309 C1. The PPS resin was dried in a through air dryer
at a temperature of 105.degree. C. to a moisture content of less
than 150 parts per million. The polymer was heated in an extruder
to 295.degree. C. The polymer was metered to a spin-pack assembly
where the melt stream was filtered and then distributed through a
stack of distribution plates to provide multiple rows of spunbond
fibers.
[0067] The spin pack assembly consisted of 4316 round capillary
openings. The spin-pack assembly was heated to 290.degree. C. and
the polymer was spun through each capillary at a polymer throughput
rate of 1.2 g/hole/min. The fibers were cooled in a cross flow
quench extending over a length of 122 cm. An attenuating force was
provided to the bundle of fibers by a rectangular slot jet. The
distance between the spin-pack to the entrance of the jet was 127
cm. The fibers exiting the jet were collected on a forming belt
traveling at 108 m/min. A vacuum was applied underneath the belt to
help pin the fibers to the belt. The spunbond layer was then passed
between an embosser roll and an anvil roll as shown in FIG. 1 to
achieve filament to filament bonding. The bonding conditions were
145.degree. C. roll temperature and 700 N/cm nip pressure. After
thermal bonding, the spunbond sheet was formed into a roll using a
winder.
[0068] The non-woven web was then smooth-calendered as in Example
1. After calendering, the spunbond sheet had a basis weight of 66
g/m.sup.2.
COMPARATIVE EXAMPLE B
[0069] In this example, a single component carded non-woven web
made from discontinuous poly(phenylene sulfide) (PPS) staple fibers
was obtained from Bondex, Inc., Trenton, S.C. The grade of material
was R073G008. A DSC spectrum of this material had an exothermic
peak of 0.5733 J/g at 122.5.degree. C., associated with the
enthalpy of crystallization of the PPS, and endothermic peak of
58.35 J/g at 281.2.degree. C., associated with the enthalpy of
fusion of the PPS. This non-woven web was then smooth-calendered as
in Example 1. After smooth calendering, the spunbond sheet had a
basis weight of 86 g/m.sup.2. A DSC spectrum of this post
calendered material had an exothermic peak of 1.064 J/g at
123.0.degree. C., associated with the enthalpy of crystallization
of the PPS, and endothermic peak of 57.59 J/g at 281.2.degree. C.,
associated with the enthalpy of fusion of the PPS. Based on the
mass of the PPS, the difference in magnitude between the enthalpy
of crystallization before calendering and the PPS enthalpy of
fusion after calendering was 57.02 J/g. A comparison between the
two DSC spectra of this example indicates that the material, as
received, was already highly crystalline and calendering did not
further increase crystallinity
COMPARATIVE EXAMPLE C
[0070] In this example, a bicomponent spunbond fabric was made from
poly(ethylene terephthalate) (PET) component and a co-polyester
(coPET) component. The PET component had an intrinsic viscosity of
0.63 dl/g and is available from E.I. du Pont de Nemours under the
tradename Crystar.RTM. polyester (Merge 4415). The coPET component
is a 17 weight percent modified di-methyl isophthalate PET
copolymer also available from DuPont as Crystar.RTM. Merge 4446.
The PET resin was dried in a through air dryer at a temperature of
120.degree. C. to a moisture content of less than 50 parts per
million. The coPET resin was dried in a through air dryer at a
temperature of 100.degree. C., to a moisture content of less than
50 parts per million. The polymers were heated in separate
extruders with the PET resin heated to 290.degree. C. and the coPET
resin heated to 275.degree. C. The two polymers were metered to a
spin-pack assembly where the two melt streams were separately
filtered and then combined through a stack of distribution plates
to provide multiple rows of spunbond fibers having sheath-core
cross sections. The PET component comprised the core and the coPET
component comprised the sheath.
[0071] The spin pack assembly consisted of 4316 round capillary
openings. The spin-pack assembly was heated to 295.degree. C. and
the polymers were spun through each capillary at a polymer
throughput rate of 0.8 g/hole/min. The PET component consisted of
70% by weight of the total weight of the spun bond fibers. The
fibers were cooled in a cross flow quench extending over a length
of 122 cm. An attenuating force was provided to the bundle of
fibers by a rectangular slot jet. The distance between the
spin-pack to the entrance of the jet was 127 cm. The fibers exiting
the jet were collected on a forming belt. A vacuum was applied
underneath the belt to help pin the fibers to the belt. The
spunbond layer was then lightly bonded between an embosser roll and
an anvil roll. The bonding conditions were 160.degree. C. roll
temperature and 700 N/cm nip pressure. After thermal bonding, the
spunbond sheet was formed into a roll using a winder.
[0072] The non-woven web was then further calendered as in Example
1 except that the line speed was 15.2 m/min, the steel roll
temperatures were 110.degree. C. and the nip pressures were 1400
N/cm. After calendering, the spunbond sheet had a basis weight of
70 g/m.sup.2.
COMPARATIVE EXAMPLE D
[0073] In this example, a commercially available non-woven web was
obtained from Innovative Paper Technologies, Tilton, N.H. The web,
marketed under the tradename ThermalShield comprised a blend of
poly(phenylene sulfide) (PPS) and poly(ethylene terephthalate)
(PET) fibers. The sheet had a thickness of 0.5 mm and a basis
weight of 44 g/m.sup.2. This non-woven was evaluated as received
without any additional smooth calendering.
[0074] Table 1 is a summary of the key parameters relating to fiber
production of the above examples and Table 2 lists the principal
non-woven web features including mechanical test results of the
webs made from these fibers.
[0075] The test results show that a calendered non-woven of PPS
sheath/PET core fibers provides an extremely low porosity web, as
measured by normalized air resistance, when compared with
comparative examples of a non sheath/core construction or a
sheath/core construction but of different polymeric components. The
mechanical properties show a similar trend.
[0076] An etched cross sectional view of this non woven web was
examined under a scanning electron microscope. The etching medium
was hexafluoroisopropanol (HFIP) which dissolved the polyester
component but left the PPS material intact. A discontinuous PPS
phase could be clearly seen.
TABLE-US-00001 TABLE 1 Fiber Production Core Sheath Fortron Hole
Average Polymer Polymer PPS Blend # of Throughput Fiber PPS/PET
Melt Point Melt Point PET Crystar % (Grade Spinning Rate Diameter
Example Ratio (Deg. C.) (Deg. C.) Merge # 0309/0317) Capillaries
(g/hole/min) (microns) 1 30/70 260 280 4415 70/30 4316 0.8 14.5 2
50/50 260 280 4415 70/30 2158 1.4 17.5 3 40/60 260 280 4415 70/30
4316 1 Not Measured 4 30/70 260 280 4434 70/30 4316 0.8 Not
Measured 5 50/50 260 280 4415 100/0 4316 0.8 16.5 6 50/50 260 280
4415 70/30 4316 1 Not Measured 7 50/50 260 280 4415 70/30 4316 1
Not Measured Comp. A 100/0 Not Known N/A N/A 100/0 4316 1.2 Not
Measured Comp. B 100/0 Not Known N/A N/A Not Known N/A N/A Not
Measured Comp. C 0/100 260 220 4415 & 4446 N/A 4316 0.8 Not
Measured Comp. D Not 260 280 N/A N/A N/A N/A Not Known Measured N/A
= Not Applicable
TABLE-US-00002 TABLE 2 Nonwoven Web Production & Evaluation
Filament Bonding Forming Roll Temp Normalized MD MD Initial Belt
Line (.degree. C.)/ Basis Air Air Elongation Tear PPS/PET Speed
Pressure Smooth Thickness Weight Resistance Resistance MD Tensile
to Break Resistance Example Ratio (m/min) (pil) Calendered
(microns) (g/m{circumflex over ( )}2) (s) (s/(g/m{circumflex over (
)}2)) Strength (N) (%) (N) 1 30/70 50.1 135/500 Yes 96 90 51 0.567
144 35.7% 25.8 2 50/50 43.8 135/500 Yes 79 78 61 0.782 138 20.1%
16.8 3 40/60 65.9 135/600 Yes 80 76 67 0.882 122 20.8% 17.6 4 30/70
52.7 135/600 Yes 80 78 34 0.436 135 33.4% 19.9 5 50/50 50.1 120/200
Yes 84 83 368 4.434 111 18.2% 16.1 6 50/50 83.4 135/500 Yes 59 53
14.1 0.266 84.8 17.2% 11.8 7 50/50 71.5 145/500 Yes 70 68 32 0.470
119 16.9% 13.3 Comp. A 100/0 108.2 145/300 Yes 100 66 0** 0.000
65.3 4.1% 11.2 Comp. B 100/0 Yes 149 86 0** 0.000 67.0 14.4% 12.3
Comp. C 0/100 Yes 131 70 0** 0.000 97.3 23.7% 19.3 Comp. D Not No
62 44 2.0* 0.045 63.2 6.8% 5.7 Known MD = Machine Direction N/A =
Not Applicable *Calculated from the time to pass 300 ml of air at a
pressure differential of 1.22 kPA. **Air resistance too low to be
measured
* * * * *