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Ekonol ® Polyester Resins

Ekonol Polyester Resin is a homopolymers based on p-oxybenzoyl repeat units, and is linear thermoplastics. Ekonol is a highly crystalline polymer but has no observed melting point even at up to 900 - 1000° F. Flow and creep are virtually non-existent below its crystal-crystal transition temperature of 625° F. Fabrication is accomplished by metallurgical techniques not normally used for polymers. The mechanical properties of Ekonol were measured on samples, which were compression sintered at 800° F and 10,000 psi. The molded polymer has a flexural strength of 5,500 psi with a modulus of 1x10 6 psi and a density of 1.44 gm/cc. Ekonol possesses a compressive strength of 15,000 psi. This high strength results in an excellent load bearing capability. Ekonol Polyesters have a thermal conductivity of 3.9 BTU/hr/ft2/° F/in. The coefficient of thermal expansion of 3.3 x 10 -5 in/in/° F is approximately linear from room temperature to 575° F. The absence of aliphatic hydrogen contributes to its excellent thermal stability in air. Ekonol undergoes a maximum weight loss of 3.5% when heated in air from room temperature to 750° F and held for 1 hour at temperature. The maximum recommended continuous service temperature is 500 - 600° F. The maximum recommended intermittent service temperature is 600 - 750° F. The dielectric constant at 10 6 Hz is 3.28 with a dissipation factor of 0.0025. Ekonol has excellent solvent resistance with the exception of concentrated sulfuric acid and strong alkalis. The water absorption rate is low at 0.4% after 500 hours at 212° F. Ekonol Polyester is self-lubricating and provides excellent friction and wear properties.

Ekonol® Linear Aromatic Polyester

O C
O
C
and wear properties. Ekonol® Linear Aromatic Polyester O C O n Flexural Strength 5500 psi Flexural

O

n
n

Flexural Strength

5500 psi

Flexural Modulus

1x10 6 psi

Thermal Conductivity

3.9 BTU / hr /ft 2 / ° F / inch

Thermal Expansion

3.3 x 10 -5 inch / inch /° F [RT to 575° F]

Transition Temperature

> 600 ° F

Molded Density

1.44 gm/cc

Dielectric Constant @ 10 6 Hz

3.28

Dissipation Factor @ 10 6 Hz

0.0025

Friction and Wear

Excellent

Solvent Resistance

Excellent except for concentrated H 2 SO 4 and strong alkalis

There are two standard products, Ekonol T101 and M102, with particle size and apparent density being the key difference. Customer runs for other average particle sizes can be completed upon request.

Typical Physical Properties

Typical Physical Properties A p p e a r a n c e : Tan -

Appearance:

Tan - Brown Powder

Form:

Highly Crystalline

Particle Size:

Screen Analysis:

Average Particle Size:

Apparent Density:

+

+

+ 325 50-85%

170

230

5% max

20% max

60 microns

10.5 grams/cubic inch

 

Typical Physical Properties

A p p e a r a n c e : Tan - White Powder

Appearance:

Tan - White Powder

Form:

Highly Crystalline

Particle Size:

Screen Analysis:

+

400

2% max

- 400

98-100%

Average Particle Size:

7 micron

Apparent Density:

3 grams/cubic inch

 

 

The polymer is highly crystalline but no melting point has been observed even at 900 – 1,000° F where the polymer decomposes rapidly. Fabrication must be accomplished below the melting point by metallurgical techniques. Ekonol powders can be converted into simple shapes or forms with compression molding techniques. More sophisticated forms and parts may require powder metallurgical techniques. In addition, surface coatings can be readily produced by plasma spray techniques. The roll of Ekonol as a filler in fabricated forms is extremely important and will be a significant part of the remainder of the information provided.

Hot Compression Molding The following has been described as the hot compression molding process used to fabricate Ekonol polymer shapes. The exact conditions will be very dependent on the molding equipment and the size of the part to be molded, use the following only as a general guideline in the development of your own process.

The basic procedure involves molding at temperatures from 550° F to 700° F and at pressures from 5,000 to 20,000 psi, and can be applied to both filled and unfilled Ekonol polymer. The material, molding equipment and the size of the part to be molded, determines exact times, temperatures and pressures.

The following procedure was developed utilizing a single action press consisting of a seven-inch ram with a 40-ton capacity. A die set was fabricated from A-20R H-13 steel hardened to 60 – 65 Rockwell C scale. Electrical heaters were built into the punches. For 100% Ekonol® polyester a temperature of 650° F is used. The hot mold is charged with either powder or a preform that has been previously dried to insure freedom from moisture. The mold is closed and low holding pressure (500 – 1,000 psi) is exerted on the powder while heating up to 650° F pressing temperature. The time required to reach the pressing temperature depends upon the thickness of the part being fabricated. When the temperature is reached, the pressure is released and the die set slightly opened to allow any volatiles to vent. The molding pressure in the range 5,000 to 20,000 is then immediately applied to the Ekonol. Depending on the size and thickness of the part, forming times of a few minutes up to an hour may be required. The pressure is then released and the part ejected from the mold. It is important to immediately place the hot part in an insulating blanket and allow it to cool slowly to below 400° F; again the time will be dependent upon the size of the part. Below 400° F the part can be cooled at any desired rate to room temperature.

Mold release compounds are not generally necessary, if needed a molybdenum disulfide aerosol is a suitable release agent. Chromed dies assist in producing a smooth surface on the part.

Lateral cracks can be caused by volatiles evolving during the pressing operation. Radial cracks can be the result of thermal stresses being set up in the pressed part, generally caused by insufficient preheat time before pressing. Extrusion of material can occur when the molding temperature is too high. Lowering the molding temperature readily corrects this problem. Dark coloration occurs when the temperature exceeds the 700° F.

Plasma Spraying Ekonol coatings can be produced by plasma spray. The Ekonol powder is fed into the plasma and the combination of heat and pressure on impact is sufficient to produce a coherent coating. Coatings can be provided on a variety of substrates.

Fillers in Fabricated Forms of Ekonol Ekonol Polyester is a very thermally stable polymer, making it easy to blend/fabricate with other high temperature materials. When combined with polytetrafluoroethylene (i.e.

PTFE); it produces a composite material that has excellent temperature and wear resistance properties. The Ekonol Polyester/PTFE blend will not wear metal surfaces and resists self-wear better than any other PTFE composition. Applications for Ekonol Polyester/PTFE blends are varied and include packing sets, compressor ring sets, "0" ring seals, spring-loaded seals, lip seals, self-lubricating bearings and rotors or vanes of process pumps. Ekonol Polyester/PTFE works best under environmentally tough conditions where wear resistance, dimensional stability and corrosion resistance are critical.

The PV, friction and wear data that will be described were obtained on two machines: the Dow Corning LFW-1 and the LWF-6 friction testers. The LFW-

1 is shown in Figure 2 and Figure

3 is a schematic of the operations. Dead weights load a stationary block against a moving ring through a compound lever system.

Figure 2

When the test ring is moved against the block, frictional force is transmitted horizontally along a tangent to the ring and may be read directly on a pressure gauge. Tests were performed using a conforming block for area contact.

Figure 3

using a conforming block for area contact. Figure 3 Figure 4 shows the Dow Corning LFW-6
using a conforming block for area contact. Figure 3 Figure 4 shows the Dow Corning LFW-6

Figure 4 shows the Dow Corning LFW-6 thrust washer-testing machine. It permits simulation of a wide variety of operating conditions and produces good reproducibility of results. Data is generated based on one surface rotating on another under predetermined loads, speeds, and environmental factors.

Figure 5 is a schematic of the LFW-6 specimen holder. It shows the rotary sample holder, stationary sample, rotary sample, torque arm and the liquid cup. With the rotary specimen moving against the stationary specimen under

torque arm and the liquid cup. With the rotary specimen moving against the stationary specimen under

Figure 4

torque arm and the liquid cup. With the rotary specimen moving against the stationary specimen under

Figure 5

predetermined conditions, the friction force can be measured with a torque gauge attached to the torque arm of the free-to-rotate stationary specimen holder. Test duration is monitored on an elapsed time meter.

The PV, friction and wear properties can be affected by a number of parameters including the percentage of Ekonol, the particle size or grade and the molding conditions. Ekonol Polyester T101 was used for all samples tested in the following discussions.

Figure 6 below shows the relative wear of Ekonol Polyester / PTFE composites versus the percent of Ekonol. The material used for these composites were DuPont Teflon® and Ekonol Polyester T101. Test pieces were preformed at 8,000 PSI and sintered at 680° F for one hour per 1/8" effective thickness (preliminary data indicated a range of preform pressures from 5,000 psi to 8,000 psi is sufficient to provide optimum properties). Duration of the test was two hours at 110 psi, 90 fpm on an LFW-1. The graph shows that the relative wear becomes asymptotic at about 25-30% Ekonol in PTFE. A blend in the range of 20 to 30% appears to be optimum for wear resistance. The value for compression molded Ekonol is approximately the same as the 50/50 blend with PTFE. This could indicate that the function of the PTFE is mainly to provide a matrix for the Ekonol particles.

Figure 6

Relative Wear vs % Ekonol in PTFE

2 hrs. Test at 110 psi, 90 fpm on LFW-1

5 10 15 20 25 30 35 40 45 50 Relative Wear
5
10
15
20
25
30
35
40
45
50
Relative Wear

% Ekonol (by Weight) in PTFE

Figure 7 shows the coefficient of friction data corresponding to the wear test in Figure 6. This graph illustrates that there is relatively little difference in the coefficient of friction between PTFE and the combination of Ekonol and PTFE. Pure Ekonol Polyester has a coefficient of friction of 0.37 under these conditions.

Figure 7

Coefficient of Friction vs % Ekonol in PTFE

Average over 2 hrs. test at 110 psi, 90 fpm on LFW-1

0 5 10 15 20 25 30 35 40 45 50 Relative Coefficient o Friction
0
5
10
15
20
25
30
35
40
45
50
Relative Coefficient o
Friction

% Ekonol (by Weight) in PTFE

The effect of sintering conditions on wear rate indicates that there is an optimum temperature for sintering as shown in Figure 8. Temperatures of 660-720° F were tried for one hour and ten hours using a 1/4" thick piece (1/8" effective thickness). We found minimum wear for pieces produced at 680° F and wear rates increased when the temperature was either raised or lowered by 20° F. At any given temperature, no improvement in wear rate was found by increasing the sintering time from one hour to ten hours. Likewise, extending the times up to 100 hours produced no significant change in wear rate. Testing was carried out on the LFW-1.

change in wear rate. Testing was carried out on the LFW-1. ! The effect of temperature

!

The effect of temperature on wear rate for Ekonol compositions is shown in Figure 9. The data indicates Ekonol is contributing resistance to wear at higher temperatures to the PTFE. The data at 500°, 550°, and 600° F are equivalent and generally represent the scatter obtained with data from the LFW-1. It should be noted that at 600° F, an increase in

Figure 9

Ekonol Compositions

Effect of Temperature on Wear Rate for

25% Ekonol in

 

PTFE

100% Ekonol

Wear (inch)* at R.T. 300° F 500° F 550° F 600° F

0.0007

0.0009

0.0013

0.0014

0.0023

0.0031

0.0019

0.0029

0.0017

0.0034

* Wear for 2 hrs test at 110 psi, 90 fpm on an LFW-1

weight loss was experienced, indicating that this temperature is approaching the upper limit of the composition.

" #

A comparison of wear rates of a 25% Ekonol in PTFE versus the three other PTFE composites is shown in Figure 10. At room temperature, the Ekonol composition provides the best wear resistance, being comparable to or slightly better than 60% bronze filled PTFE and is 2-3 times better than carbon/graphite and glass filled PTFE. At elevated temperatures, the 25% Ekonol composition is comparable with the bronze filled and carbon/graphite filled materials, and much better than the glass filled.

Figure 10

Effect of Temperature on Wear Rate for Various Teflon® Compositions

25 %

Carbon/Graphite

25%

25% Glass

60% Bronze in PTFE

 

Ekonol/PTFE

in PTFE

in PTFE

Wear (inch)* at R.T. 300° F 500° F

0.0007

0.0017

0.0022

0.0011

0.0013

0.0014

0.0026

0.0014

0.0023

0.0020

0.0041

0.0022

* Total wear for 2 hrs test at 110 psi, 90 fpm on an LFW-1

The limiting PV curve for 25% Ekonol in PTFE, as determined on the LFW-6 is shown in Figure 11. The graph indicated a limiting PV of 15,000 at 10 fpm (cold flow occurred), up to 18,000 at 100 fpm and 12,000 at 1,000 fpm (thermal runaway occurred). It can be noted the material has a limiting PV curve very similar to that of 25% carbon/graphite in PTFE.

Figure 11 Limiting PV for 25%Ekonol/PTFE

10000 1000 100 10 1 10 100 1000 Pressure (psi)
10000
1000
100
10
1
10
100
1000
Pressure (psi)

Velocity (fpm)

Figure 12 shows the wear rate for 25% Ekonol in PTFE compared to the wear rate for polyimide-filled PTFE. Duration of the test was two hours at 110 psi, 90 fpm on an LFW-1. This table shows the superior wear resistance of the Ekonol/PTFE composition at all temperatures, but especially at 500° F and above.

Figure 12

Comparison of Wear Rate for 25%

Ekonol/PTFE and Polyimide-Filled PTFE

 

25% Ekonol

Polyimide-

in PTFE

Filled PTFE

Wear (inch)** at R.T. 300° F 400° F 450° F 500° F 550° F 600° F

0.0007

0.0015

0.0013

0.0026

0.0036

0.0053

0.0023

0.0053

0.0019

0.0063

0.0017

0.0085

** Changes in thickness after 2 hrs. at 110 psi, 90 fpm on an LFW-1

The more precise frictional properties determined with 25% Ekonol in PTFE are given

in Figure 13 for a variety of environments. The tests were run on an LFW-6 at 100 fpm with a 1040 carbon steel washer. A K factor of 3x10 -10 in air makes 25% Ekonol/PTFE the lowest wearing PTFE composition available. The dynamic and static coefficients of friction are comparable to other materials. The most significant item in Figure 13 is that virtually no wear was observed for the

mating steel washer after 100 hours of testing. The same excellent wear properties were obtained in dry nitrogen and hydraulic oil; K factors of 4.5x10 -10 and 2x10 -10 respectively.

1 Approximately 100 hour test

Figure 13

Frictional Properties of 25%

Ekonol/PTFE in Various Environments

 

Air

Nitrogen (Dry)

Hydraulic Oil

K x 10 -10

3.0

4.5

2.0

C

d

0.09

0.09

0.05

C

s

0.04

0.05

0.05

Weight Loss (gm) 1 of Steel Washer

0.000

0.000

0.000

The effect of using various metals for the mating surface can be seen in Figure 14. Comparing this data to the K factor of 3x10 -10 obtained against carbon steel shows that minimal wear could be expected using brass surface. The wear against anodized aluminum is equivalent to that with the carbon steel, while cast iron and stainless steel seem to double the wear rate. If the aluminum is not anodized, the wear rate is extremely severe, both on the Ekonol/PTFE surface and on the metal surface. No scratching or weight loss of the metal washers could be detected-unanodized aluminum is the only exception.

Figure 14

K Factors for 25% Ekonol/PTFE Running against Various Metal Surfaces 1

 

Metals

K factors

1040

carbon Steel

3 x 10 -10

Brass

1 x 10 -10

304

Stainless Steel

6 x 10 -10

410

Stainless Steel

7 x 10 -10

Cast Iron

6 x 10 -10

Anodized 6063 Aluminum

3 x 10 -10

6063 Aluminum

2500 x 10 -10

1 Surface finish of 12 – 16 RMS

Typical electrical properties are shown in Figure 15. Ekonol polyester by itself is an excellent insulating material, and this is reflected in the electrical properties of the blend with PTFE. The dissipation factors are particularly good for this blend, being only slightly higher than for unfilled PTFE. Traditionally, glass-filled PTFE has been used for application where a combination of electrical and mechanical properties was required. The Ekonol filled material offers a combination of very good insulating characteristics with extremely low wear.

Figure 15

Electrical Properties

 
 

ASTM Test

Control Material

25% Ekonol

25% Fiber Glass Filled *

Property

Method

Teflon® *

in PTFE

PTFE

Dielectric Constant

D150-54T

60

cps

2.1

2.19

2.63

10 6 cps

 

2.1

2.22

2.85

Dissipation Factor

D150-54T

60

H z

0.0003

0.0007

0.0718

10 6 H z

 

0.0003

0.0005

0.0028

Volume Resistivity

D257-57T

ohm-cm

 

1 x 10 17

> 1 x 10 15

1 x 10 13

Surface Resistivity

D257-57T

ohm-cm

 

1 x 10 15

> 1 x 10 16

1 x 10 16

Arc Resistance Seconds-Tungsten Rod Method

D495

181

Dielectric Strength** v/mil

D149

350

310

300

* Typical published values

** 0.25 inch thick sample

The general physical properties for 25% Ekonol in PTFE, 20% glass in PTFE, and 100% PTFE are shown in Figure 16. The physical properties are generally comparable to those properties found in other filled PTFE compositions.

Figure 16

Typical Physical Properties

 
 

20% Fiber

 

25% Ekonol in

Glass Filled

Property

PTFE

PTFE

100% PTFE

Density Tensile Strength (psi) Strain (%) Shrinkage Hardness - Shore D Compression Strength (psi) 0.2% Offset At 1% Strain At 25% Strain

 

1.86

2.24

2.17

1800

3800

5700

180

325

450

3

2.9

3.3

63

60

57

1525

1375

1175

1275

1200

775

4700

4325

4325

Compression Modulus (psi)

13.9 x 10 4

13.6 x 10 4

8.1 x 10 4

Creep (24° C, 2000 psi, 24 hr.)

2.6%

8.5%

9.5%

Creep (100° C, 1000 psi, 24 hr.)

1.2%

3.6%

4.8%

Total Creep (24° C, 2000 psi, 24 hr.)

6.5%

12.4%

15.2%

Total Creep (100° C, 1000 psi, 24 hr.) Permanent Creep (24° C, 2000 psi,

5.4%

8.6%

14.4%

24

hr.)

3.0%

6.7%

7.0%

Permanent Creep (100° C, 1000 psi,

 

24

hr.)

1.6%

3.5%

4.6%

Coefficient of

 

Thermal Expansion (1/° C)

7.5 x 10 -5

7.2 x 10 -5

11.0 x 10 -5

(25° C - 100° C)

I I

8.4 x 10 -5

10.5 x 10 -5

11.9 x 10 -5

Thermal Conductivity (Kcal/m/hr/° C)

0.54

0.30

0.20

"

Typical chemical resistance data is shown in Figure 17.

Figure 17

Chemical Resistance of 25% Ekonol / PTFE

 
 

Temperature (°F)

Weight

Volume

Reagent

 

(30 day Exposure)

Change (%)

Change (%)

H 2 SO 4 (95%)

 

175 - 195

-24.8

0.09

HNO 3 (60%) HCl (10%)

175 - 195

-3.6

-0.17

75

-0.01

0.04

HF

(55%)

75

0.06

-0.27

AcOH (5%)

 

75

0.02

-0.49

NH 4 OH (28%) NaOH (50%) HClO (4%) Methanol Acetone

175 - 195 175 - 195 175 - 195

-26.9

-1.01

-8.8

3.63

-8.1

-0.87

75

0.01

0.25

75

0.04

0.03

CCl

4

175 - 195

0.11

0.42

The

information contained in this document is believed to be accurate and reliable but is

presented without guarantee or warranty on the part of Saint-Gobain Grains & Powders. Further, nothing presented herein should be interpreted as an authorization or inducement

to practice any patented invention without an appropriate license.