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Dispersion Guide

The document provides a comprehensive guide on DuPont Teflon® PTFE fluorocarbon aqueous dispersions, detailing their properties, applications, and processing methods. It emphasizes the importance of maintaining specific pH levels and shear stability to prevent issues like microbial growth and coagulation. Additionally, it outlines various uses of PTFE dispersions in coatings, impregnations, and blends, along with technical specifications for measuring molecular weight and particle size.

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0% found this document useful (0 votes)
15 views

Dispersion Guide

The document provides a comprehensive guide on DuPont Teflon® PTFE fluorocarbon aqueous dispersions, detailing their properties, applications, and processing methods. It emphasizes the importance of maintaining specific pH levels and shear stability to prevent issues like microbial growth and coagulation. Additionally, it outlines various uses of PTFE dispersions in coatings, impregnations, and blends, along with technical specifications for measuring molecular weight and particle size.

Uploaded by

kenneth.motz
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Technical Information

DuPont Fluoroproducts
Dispersions Properties and Processing Guide

Teflon® is a registered trademark of DuPont for its • Cast film for capacitor layer insulation and
brand of fluoropolymer resins that can only be li- diaphragms.
censed by DuPont for use in approved applications.
Customers who wish to use the Teflon® trademark, • Blends with other resins or fillers for applications
in connection with DuPont products under license such as filled bearings.
from DuPont, should contact (800) 262-2745 in • Textile finishes for yarns and fabrics, including
the U.S. and 41-22-717-5111 in Europe. Without a filter fabric.
license, customers may not identify their product as
containing Teflon®, but may refer to the resin as a • Metal coating for industrial and cookware appli-
PTFE fluoropolymer. cations. While many of the dispersions described
in this brochure can be used for metal coatings,
DuPont Teflon® PTFE fluorocarbon aqueous dis- there are formulated grades available that give
persions are milky white liquids consisting of better adhesion, abrasion resistance, and higher
submicrometer particles of tetrafluoroethylene resin build. Information on these in the United States
suspended in water. The high utility of these disper- can be obtained by calling DuPont Product Infor-
sions is due to their fluid form. This property is mation at (800) 441-7515 and asking for informa-
especially useful because DuPont Teflon® PTFE tion on “Teflon® Industrial Coatings”. In Europe,
fluorocarbon resins are not suitable for processing the phone number is 32-15-441.188 and the fax is
in molten or dissolved form. 32-15-441.160.
Dispersions based on DuPont Teflon® PFA and FEP There are also applications in which the ability of
(TFE copolymers) are also available. Unlike PTFE, PTFE to form fibrils is used. Examples of these
these dispersions are true thermoplastics and will applications include:
flow when heated above their melting points.
• Dust suppression for dusty materials such as
limestone, cat litter, catalysts, and pigments.
Uses
• Drip suppression in thermoplastics. Addition
Uses for PTFE dispersions fall into the general of PTFE dispersions to thermoplastics, along
categories of coating, impregnation, finishing, with suitable flame-retardants, allows many
and blending. More specifically the material is thermoplastics to achieve a V-0 rating in the
used for the following: UL-94 flammability test.
• Coated glass fabrics and yarns for architectural • Binders for use in either primary or secondary
applications; electrical insulation in motors, batteries.
generators, and transformers; wrapped insulation
on wire for high-temperature applications; non- The copolymer dispersions can be used either alone
adhesive separator sheets for laminating; press or in blends. They are often used as a topcoat on
blankets; gaskets, rigid high-temperature lami- coated glass fabrics to allow the fabrics to be heat-
nates; flexible wiring boards; coated glass yarn sealed together. The fabric is topcoated with FEP
overbraid in hoses; nonstick coating for platens dispersion; a piece of FEP film is placed between
in heat sealers; belting. two layers and they are then heat-sealed. Copolymer
dispersions can be blended with homopolymer
• Impregnated yarns for gasket and packing uses. dispersions to improve properties such as gloss
• Surface coatings for antistick and low friction or adhesion.
uses.

The DuPont Oval Logo, DuPont™, The miracles of science™,


Teflon®, and Zonyl® are trademarks or registered trademarks of
E.I. du Pont de Nemours and Company.
Properties of DuPont Teflon® PTFE undergoes a crystal transition at 19°C (66°F).
Fluorocarbon Dispersions PTFE is much less shear sensitive below this
PTFE dispersions are hydrophobic, negatively transition than above.
charged colloids containing particles of 0.10–0.30 µm
diameter suspended in water. DuPont Teflon® 30 Molecular Weight
and DuPont Teflon® 30B contain approximately Because of the very high molecular weight of PTFE,
60% resin, based on weight of solids. Further details the molecular weight cannot be measured by the
on the characteristics of these and other resin grades usual methods involving melt flow. Standard spe-
may be found in product sheets available from cific gravity (SSG) is the normal way to measure
DuPont. Pertinent properties are as follows. the molecular weight of PTFE. SSG is the basic
test used to measure relative molecular weight in
Surfactant homopolymer resins. The exact method is given in
PTFE dispersions, as polymerized, are very shear ASTM D4441 (sample preparation from dispersion)
sensitive. In most cases, a surfactant is added to and ASTM D4895 (molding and sintering condi-
improve the shear stability, improve wetting of sub- tions). The corresponding ISO standard is 12086.
strates, and to help with film formation in coating The basis of the test is to measure the specific grav-
operations. In most cases, a nonionic surfactant is ity of a test specimen molded and sintered under
used. Typically, these are either alkyl phenol tightly controlled conditions. The specific gravity
ethoxylates or alcohol ethoxylates. of PTFE which is 100% amorphous is 2.06 while
In a few formulations, an anionic surfactant is used. 100% crystalline PTFE has a specific gravity of
An example of this would be DuPont Teflon® PTFE 2.30. Thus, measurement of the specific gravity of
35 or 3411N, which are stabilized with the anionic the test specimen will give the percent crystallinity
surfactant sodium lauryl sulfate. if other factors such as cooling rate are held
constant. This assumes a low void content. Low
It is customary to express the amount of all addi- molecular weight PTFE will have a lower melt vis-
tives, including surfactants, as a percentage of the cosity than high molecular weight PTFE. During
PTFE resin solids: DuPont Teflon® 30 contains cooling, the lower viscosity resin will have more
60% solids and 6% surfactant. The 6% surfactant flow and, therefore, will be able to crystallize to a
is based on the PTFE solids. higher degree. This higher crystallinity will, there-
In a few cases, PTFE dispersions are used without fore, result in a higher specific gravity. Thus the
added surfactants. They only contain small amounts higher the SSG, the lower the molecular weight. The
of the surfactant used in polymerization and do not relationship between SSG and the number average
have the larger amounts of stabilizing surfactants molecular weight is:
used in most other grades. These grades will gener- SSG = 2.612 – 0.058 log10Mn
ally be mixed with other substances and then coagu-
lated to give an intimate mixture of PTFE and the SSG is a measure of molecular weight run on a
added substance (filler, pigment, etc.). sintered sample. It should not be confused with spe-
cific gravity, which is run on the liquid dispersion
These unstabilized or “raw” dispersions are ex- and is a measure of the percent solids. Typical SSG
tremely shear sensitive. They cannot be handled or values are 2.18 to 2.22 while the specific gravity
shipped like other grades without suffering from for a 60% solids dispersion is only 1.51.
excessive coagulation. These grades can be stabi-
lized in one of two ways for shipment. One method Molecular weight can also be determined using dif-
is to add a water-insoluble oil to the top of the dis- ferential scanning calorimetry (DSC). The ASTM
persions. This prevents an air/dispersion interface, standard is D4591 or ISO 11357. The initial melting
which is where coagulation occurs. The oil is then peak is between 336°C (637°F) and 345°C (653°F)
decanted away before the dispersion is used. The oil depending on the grade of resin. The heat of melting
must be completely removed or it could interfere is typically 72 J/g. The freezing peak occurs around
with coagulation. 313°C (595°F). For a grade such as Teflon® 30, the
heat of fusion will be about 35 J/g. Grades with a
The second way to stabilize the dispersion is to use lower molecular weight will have a higher heat of
liquid-full containers to eliminate the air/dispersion crystallinity because the molecules can crystallize
interface. Refrigerated shipping of these containers to a higher degree in less viscous melt. Similarly, a
(but not frozen) will add some extra shear stability. grade with a higher molecular weight than Teflon®
30 will have a lower heat of fusion (crystallization)

2
than 35 J/g. For a second heating, the melting point the frequency of equipment cleanout and disinfect
is typically 327°C (621°F) and the heat of melting is the equipment with a sodium hypochlorite solution.
about the same as the heat of fusion.
The pH should be checked periodically and, if below
For the FEP and PFA copolymers, the molecular 9, additional ammonium hydroxide should be added
weight is measured by melt flow rate (MFR). In to bring the pH into the region of 9.5–10.5. Ammo-
the MFR test (ASTM D1238 or ISO 12086-2), nium hydroxide is available in a concentrated
5 g of powder are placed in a plastometer that is reagent grade at 29% active ingredients. At this
maintained at 372°C (702°F). An orifice with a concentration, about 5 g/gal (40 g in 30-L drum)
diameter of 0.0825 inch (2.095 mm) and a length of of dispersion should suffice. Make the addition
0.315 inch (8.000 mm) is used. This orifice should slowly while stirring.
be checked before each use with a go/no-go gauge.
CAUTION
The piston is placed on the sample, which is then
allowed to thermally equilibrate for 5 min. A weight, The concentrated grade of ammonium hydroxide
usually 5.0 kg (176 oz) total, is placed on the piston can cause burns, skin irritation, and eye injury.
to extrude the resin. Cuts are taken at suitable time Use appropriate precaution against splashing,
intervals, usually 30 s. These cuts are weighed and etc., for any concentration.
normalized to 10 min flow. The higher the MFR, If necessary, for specialized applications, the pH
the lower the molecular weight. can be reduced by adding either inorganic or organic
acids, the latter are much preferred. Care must be
Particle Size taken to avoid adding excessive quantities of acid
Particle size can be determined by turbidity, by laser because high ionic strength will cause coagulation.
light scattering, ultracentrifuge, scanning Electron The dispersion should be used quickly if the pH is
Microscopy, etc. The results are reported as either in the range where microorganisms thrive (pH 4–8)
dispersion particle size (DPS) or raw dispersion to prevent souring.
particle size (RDPS). RDPS is measured before the
stabilizing surfactant is added and DPS is measured There are a few grades of DuPont Teflon® PTFE
with the surfactant present. In the older turbidity dispersions in which the pH is lower than 10.
test (ASTM D4441), there was a small difference DuPont Teflon® 35 and 3411N have a pH between
between the two methods due to the effect of the 3.5 and 5.5. This grade is stabilized with an anionic
surfactant altering the index of refraction of the surfactant that is not susceptible to attack by micro-
particle. With the newer laser methods there is little, organisms at this pH.
if any, difference between RDPS and DPS. DuPont Teflon® PTFE Grade B dispersion has a
pH of around 7 because it contains an ingredient
pH sensitive to high pH. A preservative is used in
As normally supplied, the pH of dispersions stabi- this grade to prevent attack on the surfactant by
lized with nonionic surfactants is about 10. One microorganisms.
reason for this pH is to prevent attack on the non-
ionic surfactant by microorganisms. If the pH of Shear Stability
nonionically stabilized dispersions falls below about In spite of the addition of surfactants to PTFE dis-
9, microorganisms will attack the surfactant and persions, they are still shear sensitive fluids and will
result in “sour dispersion,” named for the odor form a gelatinous coagulum if sheared excessively.
resembling spoiled milk. Under extreme conditions,
a sticky brown or black crust will form on the The preferred method of transfer of dispersion is
dispersion. flow by gravity. If pumps must be used, low shear
pumps are required. Suitable pumps are diaphragm
The pH of the dispersion is adjusted before shipment pumps, tubing or peristaltic-type pumps, disc
to about 10 with ammonium hydroxide. At this pH, pumps, and progressive cavity pumps. Centrifugal
the microorganism activity is suppressed. Ammonia pumps are high shear pumps and should be avoided.
is volatile; however, in warm weather and with use,
the ammonia level depletes and the pH drops. These All of the high molecular weight grades of PTFE
conditions eventually become favorable to microor- will fibrillate with sufficient shear and lead to a
ganism growth. If souring problems occur, increase gelatinous mixture. Maintaining the temperature
below 19°C (66°F) will reduce the tendency for

3
fibrillation. If shear stability is of great concern, It is good practice to place the impeller at an angle
consideration should be given to the use of a low to the vertical axis of the drum to achieve good mix-
molecular grade of PTFE such as Zonyl® TE 3667- ing and avoid forming a vortex that could lead to
N. This dispersion is very similar to Teflon® foaming. Normal mixing times are around 5–10 min
T-30 in particle size, percent solids, and percent depending on the impeller design, the motor speed,
surfactant. The main difference is in molecular and the amount of sediment present.
weight. The Zonyl® TE 3667-N has a much lower
The U.S. IBC has a removable 200 mm (8-in) diam-
molecular weight and is not as shear sensitive as
eter lid. For this container, either a 150 mm (6-in)
a result.
fixed impeller or a larger folding impeller can be
Zonyl® TE 3667-N is normally used as an additive used. Agitators over 230 mm (9 in) in diameter are
in other systems. The molecular weight is too low to seldom used. A 50 mm (2 in) ball valve discharge is
prevent cracking from occurring when attempting on the bottom of the container.
to cast a continuous film. Zonyl® TE 3667-N can be
The 30 L (8 gal) European container has only a
added to host systems such as paints or polishes to
50-mm (2 in) opening. To mix this drum, use a fold-
provide some of the benefits of fluoropolymers. In
ing agitator or roll the drum on the floor to mix the
some systems such as battery binders, there are
contents. While the 30-gal (113 L) US drum is also
requirements for hydrophobicity in addition to bind-
capable of being rolled, this practice is not recom-
ing ability. If used alone, a grade such as Teflon® 30
mended because the lid may be damaged in transit
may cause too much fibrillation and make the paste
and result in a leak.
unworkable. A blend of Teflon® 30 and Zonyl®
TE-3677N can be used to achieve the desired The 1000 L (264 gal) European IBC is normally
balance of binding ability and hydrophobicity. filled to only 800 L (211 gal) due to the high density
of the dispersion. The opening on the top is 150 mm
Mixing/Packaging (5.9 in) in diameter. There is a 50-mm (2 in)
It is good practice to mix the dispersion in its ship- diameter ball valve discharge on the bottom of the
ping container before removing any. This ensures container.
that the dispersion is uniform and that any re- With a 75 mm (3-in) impeller for the 113 L
dispersible sediment is incorporated. (30-gal) drum, the power of the motor should be
In the U.S., the most common shipping containers 1/4 horsepower. For the IBC, the motor should be
are a 5-gal pail, a 30-gal drum, and a 275-gal inter- 1/2 horsepower.
mediate bulk container (IBC). The U.S. drum can For either the drum or the IBC, air or electric-driven
be either an all-plastic drum or a Kraft paper drum motors can be used. Direct-driven electric motors
with a polyethylene lining. In Europe, the two most should be avoided since the usual speed is 1750
common containers are a 30-L blow-molded drum RPM, which will lead to foaming. Gear-driven elec-
and a 1,000-L IBC. tric motors normally operate at 350 RPM and are
The 30-gal US container is equipped with a fully suitable for mixing. Variable speed electric motors
removable plastic lid. There is also a 2-in bung offer more flexibility than the gear-driven electric.
opening. To agitate the drum the lid is removed or a Air motors are variable speed motors and are
folding impeller stirrer is inserted through the bung. acceptable if flammable ingredients are present.
Removing the lid allows the condition of mixing to
be observed, while inserting a folding impeller Filtration
through the bung minimizes the chances for con- Although the dispersion products have been filtered
tamination. Typically a 80 or 100 mm (3- or 4-in) at the time of manufacture, it is good practice to
impeller is used. Many styles of impeller are used. filter the dispersions again before use, particularly
The turbine design is preferred because it provides if the dispersion has been previously used. Filter
good mixing with a low power requirement and is sizes can range from simple cheesecloth to very fine
low in shear. The impeller should be placed about 10-µm (0.4 mil) filters depending on the application
150 mm (6 in) from the bottom of the drum for best involved. For most purposes, a 50- or 75-µm (2- or
results. Under no circumstances should the impeller 3-mil) filter is sufficient.
be immersed in the sediment, as this will result in
shearing of the sediment.

4
The filter media can be woven fabric, a felted fabric, Table 1
or even woven wire mesh. Suitable materials of Typical Values
construction are stainless steel, polypropylene,
polyester, or nylon. These filters can be in the form Grams Pounds of
Percent Specific Solids Solids
of metal baskets, woven cartridges, or bags.
Solids Gravity per Liter per Gallon
A filter can also be used to remove any foam that
35 1.24 436 3.72
may be present.
40 1.29 515 4.30
Storage Conditions 45 1.34 601 5.01
For most grades, acceptable storage conditions are 50 1.39 693 5.79
7–32°C (45–90°F). Preferred conditions are 7–24°C 60 1.50 900 7.50
(45–75°F). In general, storage at 7°C (45°F) will
halve the sedimentation rate obtained at room tem- A more complete table for the relationship between
perature. Storage at 32°C (90°F) will have about specific gravity and percent solids for PTFE is given
twice the sedimentation rate as at room temperature. in Table 2 at the end of this bulletin.
Stirring or rolling the containers once per month
can significantly extend the shelf life. Freezing Critical Cracking Thickness
must be avoided because it will result in irreversible The critical cracking thickness (CCT) is the maxi-
coagulation. mum thickness of coating that can be made in a
The one exception to the storage temperature single casting without formation of cracks when the
recommendation is with DuPont Teflon® Type 35 deposited polymer is dried. The critical cracking
and 3411N. These grades are stabilized with thickness can range from as low as 2 µm (0.08 mil)
sodium lauryl sulfate and this surfactant becomes up to 20 µm (0.8 mil), depending on the grade of
less soluble as the temperature is decreased. Pre- dispersion used, the application conditions, and the
ferred storage conditions are 55–75°F (12–24°C) shape being coated. Thus, coatings no thicker than
to maintain solubility of the surfactant. 2 µm (0.08 mil) to 20 µm (0.8 mil) are usually de-
posited in a single cycle to avoid forming cracks
As dispersion ages, some sediment will form result- that cannot be fused together in sintering. Multiple
ing in a loss of PTFE solids. The percent solids in dipping and sintering operations make thicker
dispersion can be estimated by measuring specific coatings.
gravity and using the relationship in Table 2
between specific gravity and percent solids. This Formulations
will give a good indication if settling has become
Most DuPont Teflon® PTFE fluorocarbon dis-
excessive.
persion, as furnished, contains a nonionic wetting
As the PTFE solids settle out of suspension, the agent with good wetting properties and a minimum
surfactant (because it is expressed as a percentage tendency to foam. The wetting agent can be decom-
of the PTFE solids) will increase. This could lead posed at the temperatures required for baking, mini-
to an increased viscosity or to poor color due to the mizing residual contamination.
excess surfactant. The solids and surfactant level
can be accurately measured in a gravimetric test. In some cases, it may be desirable to supplement
Approximately 10 g (0.3 oz) of dispersion is the formulation by diluting or by using additives
weighed into a tared aluminum pan. The sample is to adjust properties.
dried at 120°C (248°F) for 2 hr to remove the water. In other cases, it may be desirable to increase the
The pan is then placed in an oven at 380°C (716°F) viscosity of the dispersion. This is done to either
for 35 min to remove the surfactant. From these increase the build per pass or to keep additives sus-
weights, the percent PTFE and percent surfactant pended. The viscosity may be increased by adding
can be calculated. Details are in ASTM D4441 or water-soluble thickeners such as alkali-soluble
ISO 12086. acrylics, acrylic acid copolymers, or cellulose de-
High-speed stirring and addition of electrolytes or rivatives. Examples are Acrysol® GS and Acrysol®
water-miscible solvents will also usually lead to ASE-75 (Rohm & Haas Co.) or Carbopol® 934
irreversible coagulation. (B. F. Goodrich Co.). As little as 0.1% of
Carbopol® 934 will increase the viscosity of a
Specific Gravity 60% solids dispersion to 600 cP (mPa•s).
The relationship between concentration and specific
gravity at 25°C (77°F) is given in Table 1, along with
useful equivalents.

5
Nonionic and anionic types of surfactants are also Film Casting and Coating
useful for increasing the viscosity. The nonionic The availability of DuPont Teflon® PTFE resins in
wetting agents are generally preferred because they the form of aqueous dispersions makes it possible to
can be burned out more readily at polymer-sintering cast films and to apply enamel-type coatings of the
temperatures without leaving inorganic residues in material. In the case of coatings, DuPont Teflon®
the product. It is important that only mild agitation PTFE dispersion is applied by dipping or flowing
be used when adding material to the dispersion. onto the surface, followed by drying to remove
High-speed stirring can lead to coagulation. water (or other media, in the case of some finishes),
Addition of 1.5% Triton® X-45 (Union Carbide) and fusing the dried polymer at 360°C (675°F) to
can increase the viscosity of Teflon® 30 from 20 cP 400°C (750°F). Dip coating has proved preferable
to 405 cP. in most cases because of its adaptability to continu-
ous application of a uniform coating. A dispersion
Long-chain fatty alcohols and amine can also be concentration of 45–50% solids by weight and
used to thicken dispersion. As an example, 2.8% 6–9% (on solids basis) wetting agents are recom-
dodecanol will increase the viscosity of Teflon® 30 mended for optimum wetting characteristics. The
from 20 cP to 200 cP. Dodecyl amine is even more thickness of dispersion layer picked up during each
effective; 0.25% will increase the viscosity of dip should be limited to about 12 µm (0.5 mil) to
Teflon® 30 to 980 cP. avoid cracks upon drying as well as to permit vapor-
The viscosity of many of these thickened dispersions ization of the dispersing agent during the sintering
will be non-Newtonian, i.e., the apparent viscosity operation. Thicker coatings can be applied in a
will decrease with increasing shear rate. The viscos- single pass if high dielectric strength is not needed.
ity of a thickened dispersion was measured using a The viscosity of the dispersion, the coating speed,
Brookfield viscometer operated at different spindle and the roughness of the surface being coated influ-
speeds to vary the shear rate. The results are shown ence the amount of pickup, but it can be controlled
below. by means of a doctor knife or wire-wrapped wiper
bars for flat surfaces. As many coats may be ap-
Spindle Speed Apparent Viscosity plied as desired. It is not unusual for a coat to be
RPM cP (mPa•s) sintered before another coat is applied.
60 172 After dipping, the next step is removal of the water
30 263 from the deposited dispersion. This may be done
12 505 under infrared lamps or in a forced-convection air
oven. In either case, the speed of water removal will
6 725
be limited by the tendency for bubble formation. For
3 1,220 a 25 µm (1-mil) coating, infrared drying will take
1.5 1,900 about 15 s. The air-oven technique will take as long
as 1–2 min at 85–96°C (185–205°F).
With some thickened dispersions, some phase sepa- A drying, baking, and sintering operation is used
ration may occur due to depletion flocculation. during which the wetting agent is volatilized follow-
Thickened dispersions that have been allowed to ing drying and the resin particles are sintered into a
stand for several days may show a clear upper layer. homogeneous film. Both operations can be carried
This dispersion is still redispersible. Different thick- out simultaneously at the sintering temperature.
eners will show this effect to different degrees. However, it is recommended that the baking step
Separation is more likely to occur when the vis- be conducted separately at a lower temperature to
cosity is between about 75–400 cP. Above this minimize the decomposition of the wetting agent to
level, the dispersion is usually too viscous for phase a carbonaceous residue. Baking or volatilization of
separation to occur. the wetting agent is carried out in an air oven main-
The surface tension of most grades of DuPont tained at a temperature of about 288°C (550°F).
Teflon® is about 32 dyn/cm. This is sufficient to wet Temperatures of 260–316°C (500–600°F) are most
most surfaces. If wetting problems are encountered, commonly used, depending on the equipment and
additional wetting agents can be added. Additional desired baking time.
Triton® X-100 (Union Carbide) often will improve
wetting even though additional amounts do not sig-
nificantly affect the surface tension. If lower surface
tension is desired, a surfactant such as Silwet® L-77
(Witco) can be added. Normally, 0.5–1.0% is added
based on PTFE solids.

6
Sintering or fusion of the resin particles takes place be removed by heating to about 290°C (550°F).
almost instantaneously on reaching temperatures of The required time will be a matter of a few minutes.
360–400°C (675–750°F). Most of the wetting agent Lower temperatures and longer times can be used
is volatilized at the baking temperature; however, a when impregnating fibers with low thermal stability.
small amount remains and decomposes during sin- Pressure is usually applied to the impregnated mate-
tering, leaving a minute carbonaceous residue that rial, either before or after drying, to aid in holding
can be removed by oxidation if the sintering time the Teflon® resin in place. For example, a fabric or
is extended. Whether or not this residue should be material can be calendered continuously as an inte-
baked out depends on the application; it causes dis- gral part of the treatment, or the dried material
coloration, detracts from the electrical properties, can be compressed in a mold as an after-treatment.
and makes film stripping very difficult. If these are Thus, in addition to glass and asbestos, less heat-
not important factors, the sintering cycle can be resistant fibers can also be treated.
relatively short—about 3 min for a 25 µm (1-mil)
coating. However, for complete removal of stabi-
lizer residues, a sintering cycle of about 8–10 min Glass Fabric Coating
is preferred for a 25 µm (1-mil) coating. The Typical equipment for impregnating and coating
cycle increases to about 30 min for a 50 µm (2-mil) glass cloth with DuPont Teflon® PTFE dispersion
coating. Hence, multiple applications and sintering is shown in Figures 1, 2, and 3. Each includes:
of 25 µm (1-mil) each are more desirable from the • Payoff roll for the cloth
standpoint of sintering time, even if the critical
thickness was great enough to permit thicker depos- • Dip tank for the dispersion
its in a single cycle. Multiple dips, with baking and • Drying and sintering zone
sintering between dips, result in good homogeneity.
• Take-up roll
The copolymer dispersions are usually processed
at a lower temperature because they have lower The dip tank should be constructed of stainless steel.
melting points. FEP has a melting point around The tank should be equipped with at least one sub-
265°C (509°F) and is normally processed between merged rigid rod. If rotating rolls are used, the roll
300–350°C (572–662°F). PFA has a melting point must be entirely submerged. On some products,
of 305°C (581°F), and is normally processed multiple submerged dip rolls have resulted in im-
between 340–370°C (645–700°F). proved face-to-back coating pickup uniformity and
improved impregnation. For applying first coats on
very heavy fabrics, a partially submerged roll
Impregnation (sometimes engraved) at the dip tank entrance forces
A variety of porous structures can be impregnated dispersion through the thickness of the fabric. For
with PTFE dispersion. The dispersion is well-suited some products, the forced displacement of air can
for impregnation because of its low viscosity, result in noticeable improvement in impregnation.
extremely small particles and the effect of the
surfactant, which aids in wetting the surfaces of Figure 1 represents a minimum cost, first generation
interstices and promotes capillary action. After design that can still be effectively used on a limited
dipping and drying, the deposit of resin may or product line. Only one temperature-controlled heat
may not be sintered depending on the requirements exchanger is required for the sintering zone. The
of the application. drying and baking areas occur from natural cooling
as a result of the introduction of makeup air just
Sintered coatings on woven fabrics and mats of below the recirculating duct. Limited control of the
glass are a matter of casting films on a discontinu- temperature profile in the drying/baking zone is
ous surface. Due to the critical thickness factor, achieved by sliding doors to vary the size of the
multiple dips, usually with sintering between dips, opening for admitting makeup air and by varying
are essential to build heavy coatings of good homo- the ratio of the exhaust to the recirculating air.
geneity.
More sophisticated units are shown in Figures 2
Impregnated materials with a useful degree of and 3. Three independently controlled temperature
chemical resistance and the nonadhesive property zones are used; the first for “drying” (slow removal
of DuPont Teflon® PTFE can be prepared without of water without blistering), the second for “baking”
sintering the deposited polymer. This involves (removal of organic wetting agent), and finally a
merely dipping and drying. The wetting agent may sintering zone. The accumulator and turret rewind

7
can be used with any design to achieve continuous Applicators can be used to wipe excessive coatings
operation without stopping for roll changes. The from the fabric. Types of applicators are listed in
design shown in Figure 3 can be used where head order of decreased amount of wiping (increasing
room is limited or as a means of limiting the tension pickup at any given speed):
applied to the machine direction of heavyweight • Sharp-edged knives
fabrics by minimizing the length (and thus the
weight) of fabric in the vertical direction. The • Round-edged knives
“crimp” interchange between warp and fill yarns, • Wire-wound rods
when excessive tension is applied to the machine
direction, can be destructive to mechanical strength • Horizontally opposed, spring-loaded fixed gap
properties in the fill direction of the coated fabric. metering rolls
• No applicators

Figure 1. Simple Countercurrent Tower

Exhaust

Bake Heat
and Exchanger
Sinter

Makeup Air Ports


(Sliding Doors)
Dry
and Exhaust
Bake Fan

Tension Rolls

Optional
Multiple
Dip Rolls

Side View Front View

8
Figure 2. Modern Coating Tower at least some of the coats but dilution to 50–55%
solids is more normal. This reduces the viscosity
Countercurrent Flow Each Zone or and allows the dispersion to wick into the fabric
Direct Impingement Slot Dryers or better and displace air. Coating speed per pass can
Radiant Heat: Separate Exhausts Each Zone vary from 0.3–13.7 m/min (1–45 ft/min). Each
CAUTION: Keep air velocities low to avoid coat must be below the critical cracking thickness
fabric flutter and excessive tension to avoid mud cracking. Alternately, if several
unsintered coats are applied, the coated fabric
should be calendered prior to sintering to seal mud
cracks. This equipment is, typically, a chrome-
plated steel roll with a compressed paper backup
roll. A temperature of about 175°C (350°F) and a
pressure of about one ton per linear inch width is
a good starting point for optimizing this operation.
Sinter
370–420˚C
Wetting agent removal during baking must be com-
plete to avoid coating pick off during calendering.
Calendering of unsintered coating at an intermediate
stage is also useful in flattening and burying glass
filament defects into the soft coating early in the
process. Without the calendering operation, these
filament defects can result in lumps in the coated
Bake
200–315˚C fabric surface or result in channels to wick moisture
and reduce the electrical properties of electrical
grade-coated fabrics.

Lamination
Standard laminating presses can be used for the
Dry production of laminates of glass cloth coated with
30–100˚C DuPont Teflon® PTFE. Presses should be equipped
with electrically-heated platens, which are capable
of heating the coated glass cloth to a temperature
of about 400°C (750°F) and have sufficient tonnage
Applicators to apply up to 6.9 MPa (1,000 lb/in2). The platens
should be cored for cooling water so that the lami-
nates can be cooled under pressure. Cooling the
laminate under pressure helps to reduce warp and
twist in the finished laminate. Separate presses or
a multiple opening press with hot and cold platens
can be used to avoid the necessity of repeated heat-
ing and cooling of a single opening press.
Cutting the cloth to the desired sizes, tacking the
Ventilating ducts and an exhaust blower to remove cut pieces by hand, pressing the assembly between
volatile products and traces of decomposition heated platens, and cooling makes laminates of
products from the ovens should be used (see Safe coated glass cloth. It is important that the individual
Handling Practices). layers be flat and that there be no wrinkles before
pressure is applied. Pressure should be applied
Glass Greige Goods that contain approximately slowly so that air, which will expand during heat-
1–2% of a starch-oil size are most commonly used ing and cause blisters, will not be entrapped.
for impregnation. In special cases, other finishes on
the glass may be employed. There is some tendency for the DuPont Teflon®
PTFE resins to stick to heated metal platens during
Depending on the fabric weave and thickness de- lamination. To eliminate this, a foil of aluminum
sired, anywhere between one to twelve coats might can be placed on both the top and bottom of the
be required. Bath compositions will also vary with lay-up. Silicone mold releases are helpful. After
the type of fabrics and the coating speeds. Some removal of the laminate from the press, the foil
operations use undiluted 60% solids dispersion for can be stripped off easily.

9
Figure 3. Modern Coating Tower—For Use Where Head Room Is Limited

Alternate
Air Cushion Rolls

Bake
200–315˚C

Sinter
370–420˚C
Dry
30–100˚C

Accumulator

Turret Rewind
Optional: Multiple Rolls in Dip Tank

It is important that the platens be parallel so that Safe Handling Practices


pressure will be applied equally to all sections of the Industrial experience in the handling of fluoropoly-
laminate. Chrome-plated platens or polished press mer resins is extensive. Large quantities of these
plates are generally used to prevent rusting and to resins have been processed safely by many fabrica-
impart a good surface to the finished laminate. tors in a variety of processes. The record clearly
Normal laminating pressures and temperatures are establishes that fluoropolymer resins can be pro-
3.4–6.9 MPa (500–1,000 lb/in2) and 360–427°C cessed and used safely.
(680–800°F), respectively. Although pressures are not The “Guide to the Safe Handling of Fluoropolymer
critical, the pressure must be great enough to squeeze Resins,” latest edition, published by the Fluoro-
residual air out and to force the individual layers of polymers Division of The Society of the Plastics
coated cloth into intimate contact. The heat must be Industry or in Europe the “Guide for the Safe Han-
applied at temperatures above 327°C (621°F) for a dling of Fluoropolymer Resins” published by APME
sufficient period of time to fuse all of the PTFE resin are available through DuPont and provide guidelines
throughout the thickness of the laminate. for the safe handling and use of fluoropolymers in
a variety of situations. These include varying tem-
Blends peratures, skin contact, ingestion, scrap disposal,
Homogeneous mixtures of DuPont Teflon® machining, reactivity toward certain chemicals,
polytetrafluoroethylene resins with a variety of ma- and medical uses. It is essential to follow instruc-
terials can be prepared from the dispersion. Broadly, tions in these booklets when working with fluoro-
the procedure is simply a matter of mixing the mate- carbon resins.
rial to be blended into the dispersion. Solid materials
Before using fluoropolymer dispersions or resins,
should be in a finely divided state. Best results will
read the Material Safety Data Sheet corresponding
usually be obtained by suspending the solid in water
to those particular products.
before mixing slowly with the dispersion. Systems
in immiscible liquids can frequently be processed Periodic inspections are recommended to ensure that
through the use of mutually miscible solvents such as the ventilation and handling equipment is adequate
acetone or alcohol, though coagulation of the solid and in good, safe working order.
resin particles will occur immediately on mixing.

10
Table 2
Relationship Between Specific Gravity and Percent Solids for PTFE Dispersions
Valid for PTFE with an inherent polymer density of 2.285 g/cm3 and containing 6% of a wetting agent with a density
of 1.067 g/cm3 at 25ºC (77ºF)

0 1 2 3 4 5 6 7 8 9

1.09 14.58% 14.73% 14.88% 15.03% 15.18% 15.32% 15.47% 15.62% 15.77% 15.91%
1.10 16.06% 16.20% 16.35% 16.49% 16.64% 16.78% 16.93% 17.07% 17.22% 17.36%
1.11 17.50% 17.65% 17.79% 17.93% 18.08% 18.22% 18.36% 18.50% 18.64% 18.78%
1.12 18.93% 19.07% 19.21% 19.35% 19.49% 19.63% 19.77% 19.91% 20.04% 20.18%
1.13 20.32% 20.46% 20.60% 20.74% 20.87% 21.01% 21.15% 21.28% 21.42% 21.56%
1.14 21.69% 21.83% 21.96% 22.10% 22.23% 22.37% 22.50% 22.64% 22.77% 22.91%
1.15 23.04% 23.17% 23.31% 23.44% 23.57% 23.70% 23.84% 23.97% 24.10% 24.23%
1.16 24.36% 24.49% 24.63% 24.76% 24.89% 25.02% 25.15% 25.28% 25.41% 25.54%
1.17 25.67% 25.79% 25.92% 26.05% 26.18% 26.31% 26.44% 26.56% 26.69% 26.82%
1.18 26.94% 27.07% 27.20% 27.32% 27.45% 27.58% 27.70% 27.83% 27.95% 28.08%
1.19 28.20% 28.33% 28.45% 28.58% 28.70% 28.82% 28.95% 29.07% 29.19% 29.32%
1.20 29.44% 29.56% 29.68% 29.81% 29.93% 30.05% 30.17% 30.29% 30.41% 30.54%
1.21 30.66% 30.78% 30.90% 31.02% 31.14% 31.26% 31.38% 31.50% 31.61% 31.73%
1.22 31.85% 31.97% 32.09% 32.21% 32.33% 32.44% 32.56% 32.68% 32.80% 32.91%
1.23 33.03% 33.15% 33.26% 33.38% 33.50% 33.61% 33.73% 33.84% 33.96% 34.07%
1.24 34.19% 34.30% 34.42% 34.53% 34.65% 34.76% 34.87% 34.99% 35.10% 35.21%
1.25 35.33% 35.44% 35.55% 35.67% 35.78% 35.89% 36.00% 36.11% 36.23% 36.34%
1.26 36.45% 36.56% 36.67% 36.78% 36.89% 37.00% 37.11% 37.22% 37.33% 37.44%
1.27 37.55% 37.66% 37.77% 37.88% 37.99% 38.10% 38.21% 38.32% 38.42% 38.53%
1.28 38.64% 38.75% 38.85% 38.96% 39.07% 39.18% 39.28% 39.39% 39.50% 39.60%
1.29 39.71% 39.82% 39.92% 40.03% 40.13% 40.24% 40.34% 40.45% 40.55% 40.66%
1.30 40.76% 40.87% 40.97% 41.08% 41.18% 41.28% 41.39% 41.49% 41.59% 41.70%
1.31 41.80% 41.90% 42.01% 42.11% 42.21% 42.31% 42.41% 42.52% 42.62% 42.72%
1.32 42.82% 42.92% 43.02% 43.12% 43.23% 43.33% 43.43% 43.53% 43.63% 43.73%
1.33 43.83% 43.93% 44.03% 44.13% 44.23% 44.32% 44.42% 44.52% 44.62% 44.72%
1.34 44.82% 44.92% 45.01% 45.11% 45.21% 45.31% 45.41% 45.50% 45.60% 45.70%
1.35 45.79% 45.89% 45.99% 46.09% 46.18% 46.28% 46.37% 46.47% 46.57% 46.66%
1.36 46.76% 46.85% 46.95% 47.04% 47.14% 47.23% 47.33% 47.42% 47.52% 47.61%
1.37 47.71% 47.80% 47.89% 47.99% 48.08% 48.17% 48.27% 48.36% 48.45% 48.55%
1.38 48.64% 48.73% 48.82% 48.92% 49.01% 49.10% 49.19% 49.29% 49.38% 49.47%
1.39 49.56% 49.65% 49.74% 49.83% 49.92% 50.02% 50.11% 50.20% 50.29% 50.38%
1.40 50.47% 50.56% 50.65% 50.74% 50.83% 50.92% 51.01% 51.10% 51.18% 51.27%
1.41 51.36% 51.45% 51.54% 51.63% 51.72% 51.81% 51.89% 51.98% 52.07% 52.16%
1.42 52.24% 52.33% 52.42% 52.51% 52.59% 52.68% 52.77% 52.86% 52.94% 53.03%
1.43 53.11% 53.20% 53.29% 53.37% 53.46% 53.55% 53.63% 53.72% 53.80% 53.89%
1.44 53.97% 54.06% 54.14% 54.23% 54.31% 54.40% 54.48% 54.57% 54.65% 54.73%
1.45 54.82% 54.90% 54.99% 55.07% 55.15% 55.24% 55.32% 55.40% 55.49% 55.57%
1.46 55.65% 55.74% 55.82% 55.90% 55.98% 56.07% 56.15% 56.23% 56.31% 56.39%
1.47 56.48% 56.56% 56.64% 56.72% 56.80% 56.88% 56.96% 57.05% 57.13% 57.21%
1.48 57.29% 57.37% 57.45% 57.53% 57.61% 57.69% 57.77% 57.85% 57.93% 58.01%
1.49 58.09% 58.17% 58.25% 58.33% 58.41% 58.49% 58.56% 58.64% 58.72% 58.80%
1.50 58.88% 58.96% 59.04% 59.11% 59.19% 59.27% 59.35% 59.43% 59.50% 59.58%
1.51 59.66% 59.74% 59.81% 59.89% 59.97% 60.05% 60.12% 60.20% 60.28% 60.35%
1.52 60.43% 60.50% 60.58% 60.66% 60.73% 60.81% 60.89% 60.96% 61.04% 61.11%
1.53 61.19% 61.26% 61.34% 61.41% 61.49% 61.56% 61.64% 61.71% 61.79% 61.86%
1.54 61.94% 62.01% 62.09% 62.16% 62.24% 62.31% 62.38% 62.46% 62.53% 62.60%
1.55 62.28% 62.75% 62.82% 62.90% 62.97% 63.04% 63.12% 63.19% 63.26% 63.34%
1.56 63.41% 63.48% 63.55% 63.63% 63.70% 63.77% 63.84% 63.91% 63.99% 64.06%

Example: A SG of 1.514 corresponds to 59.97% solids

11
For more information on Fluoroproducts: (302) 479-7731
North America
DuPont Fluoroproducts
P.O. Box 80713
Wilmington, DE 19880-0713
www.teflon.com

Europe Japan Asia Pacific


DuPont de Nemours Int’l SA DuPont Mitsui Fluorochemicals DuPont China, Limited
DuPont Fluoroproducts Co., Ltd. 1122 New World Office Bldg.
2, chemin du Pavillon Chiyoda Honsha Building (East Wing)
P.O. Box 50 5–18, Sarugaku-cho 1-chome 24 Salisbury Road
CH-1218 Le Grand-Saconnex Chiyoda-ku, Tokyo 101 Japan Tsim Sha Tsui
Geneva, Switzerland 81-3-5281-5872 Kowloon
Tel +41(0)227175111 Hong Kong
Telefax +41(0)227175411 (852) 27341948
[email protected]

Canada South America


DuPont Canada, Inc. DuPont do Brasil S/A
DuPont Fluoroproducts Fluoropolymers
P.O. Box 2200, Streetsville Alameda Itapecuru, 506
7070 Mississauga Road 06454-080 - Alphaville
Mississauga, Ontario, Canada P.O. Box 263
L5M 2H3 Barueri, Sao Paulo, Brazil
(905) 821-5194 0800-171715
[email protected]

The information set forth herein is furnished free of charge and is based on technical data that DuPont believes to be reliable. It is intended for use by persons
having technical skill, at their own discretion and risk. The handling precaution information contained herein is given with the understanding that those using
it will satisfy themselves that their particular conditions of use present no health or safety hazards. Because conditions of product use are outside our control,
we make no warranties, express or implied, and assume no liability in connection with any use of this information. As with any material, evaluation of any
compound under end-use conditions prior to specification is essential. Nothing herein is to be taken as a license to operate under or a recommendation to infringe
any patents.
CAUTION: Do not use in medical applications involving permanent implantation in the human body. For other medical applications, see “DuPont Medical
Caution Statement,” H-50102.

(10/01) RWJ86 Printed in U.S.A.


[Replaces: E-55514-2]
Reorder No.: H92067

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