This technical paper was written and developed in August, 1993 when the author(s) was an employee of Dyneon LLC. Dyneon LLC was formerly a wholly-owned subsidiary of 3M Company and was fully integrated into 3M Company on January 1, 2011. Title: The Influence of Polymer Processing Additives on The Surface, Mechanical, and Optical Properties of LLDPE Blown Film Abstract: Linear Low Density Polyethylene (LLDPE) film was blown from both wide and narrow die gaps, with and without two commercial polymer processing additives. Wide die-gap extrusion was used to determine how the physical presence of either processing additive affected various mechanical and optical properties of the resultant films. Narrow die-gap extrusion demonstrated how polymer processing additives can be utilized to improve extrusion parameters and permit production of films with improved properties. Finally, all films were analyzed, both prior to and after corona treating, and monitored over a one year period to determine if either processing additive influenced the surface chemistry, surface morphology, or wettability of the films. Keywords: Blown Film, Corona Discharge, ESCA, Linear Low Density Polyethylene, Melt Fracture, Physical Properties, Polymer Processing Additive, Surface Chemistry, Wettability

Date Published: August, 1993

The Influence of Polymer Processing Additives on The Surface, Mechanical, and Optical Properties

of LLDPE Blown Film

By

T.J. Blong, D.F. Klein A. V. Pocius, M.A. Strobel

3M Specialty Fluoropolymers Department

3M Center St. Paul, Minnesota 55144-1000

No. 12

THE INFLUENCE OF POLYMER PROCESSING ADDITIVES ON THE SURFACE, MECHANICAL, AND OPTICAL PROPERTIES OF LLDPE BLOWN FILM

Thomas J. Blong 3M, Specialty Fluoropolymer Department St. Paul, Minnesota, USA 55144-1000

A. V. Pocius 3M, Adhesive Technologies Center

ABSTRACT

Donald F. Klein 3M, Specialty Fluoropolymer Department

Mark Strobel 3M Corporate Research Process Technology Lab

Linear Low Density Polyethylene (LLDPE) film was blown from both wide and narrow die gaps, with and without two commercial polymer processing additives. Wide die-gap extrusion was used to determine how the physical presence of either processing additive affected various mechanical and optical properties of the resultant films. Narrow die-gap extrusion demonstrated how polymer processing additives can be utilized to improve extrusion parameters and permit production of films with improved properties. Finally, all films were analyzed, both prior to and after corona treating, and monitored over a one year period to determine if either processing additive influenced the surface chemistry, surface morphology, or wettability of the films.

KEYWORDS

Blown Film, Corona Discharge, ESCA, Linear Low Density Polyethylene, Melt Fracture, Physical Properties, Polymer Processing Additive, Surface Chemistry, Wettability

INTRODUCTION

The use of fluorocarbon based polymer processing additives (PPAs) for the elimination of melt fracture in linear polyethylenes (1) has become well established in the film industry. Likewise, the relationship of this additive with other common polyolefin additives has been intensively researched and documented (2-6).

Although it has been shown that these materials can improve the economics of blown film production (7), and be used to improve certain properties (8), sparse information and data are available on the effect of their physical presence in the film after fabrication. With that in mind, experiments were conducted to assess the impact of polymer processing additives on film characteristics such as surface chemistry, morphology and wettability, and mechanical and optical properties.

EXPERIMENTAL

Materials

The two commercial polyolefin resins used are listed in Table 1. The first, referred to as LLDPE-1, was a 1.0 melt index, 0.918 density, 1-hexene copolymer resin. LLDPE-2, a 2.0 MI, 0.918 density, 1-butene copolymer, was used as the PPA masterbatch carrier resin. Both resins contained an anti-oxidant package, but no slip or anti-block additives.

The PPAs used in this study were based on fluorocarbon polymers. The two products used, FX-9613 and FX-5920, are commercially available as free-flowing powders and will

hereafter be referred to as PPA-1 and PPA-2. The latter was designed for processing

improvements in systems containing inorganic fillers, pigments, and anti-blocking agents (4,5,6). It also shows improved performance in unfilled systems.

Masterbatches of PPA-1 and PPA-2 were obtained commercially at 3% levels compounded in LLDPE-2. The concentrates were analyzed for final concentration and dispersion quality by 3M test methods (9,10).

Equipment and Sample Preparation

The desired final process additive levels were obtained by pre-blending the required quantity of PPA masterbatch with the host polymer in a tumble blender for a minimum of 20 minutes. To compensate for any effects from the concentrate carrier resin, an equal amount of the neat LLDPE-2 was added to the control samples.

Films for mechanical and optical testing were produced using an 89 mm Davis Standard extruder with a 24/1, length to diameter (UD) barrier screw. Extrusion conditions are listed in Table 2. The die was of spiral design, with a diameter of 20.3 cm. Die gaps of 1.0 and 2.3 mm were used. A dual lip air ring with chilled air provided cooling and bubble stability. For each formulation, extruder readings were recorded, and film samples collected, at the end of one hour to ensure that the system was at equilibrium.

Films for surface analysis were produced using a Kiefel blown film line with a 40 mm, 24/1 : UD, grooved feed extruder. The die was also of spiral design, with a diameter of 80 mm. Die gaps of 0.6 and 2.0 mm were used. An adjustable single lip air ring with chilled air was used for cooling. An iris and sizing cage provided further bubble stability. Details of the extrusion conditions are listed in Table 3. Film was produced with a nominal gauge of 25 microns.

These films were corona treated using an industrial "covered-roll" corona treater from Sherman Treaters Ltd. It was equipped with a 4 kW power supply from ENI Power Systems Inc. Films were treated at 0.93 J/cm2, at the ambient air temperature, with a measured humidity of 8%. Treatment parameters were chosen such that a nominal surface energy of 48 dynes/cm was achieved, as measured by the ASTM wetting test (11).

ANALYTICAL METHODS

Physical property measurements were performed by a contract lab, according to the ASTM standards cited in Table 4.

Measurements of the advancing, (9a) and receding, (9r) contact angles in air of distilled, deionized, and filtered water were made on a Rame-Hart contact goniometer.

The film samples were also analyzed by SSIMS (Static Secondary Ion Mass Spectroscopy) (12) and ESCA (Electron Spectroscopy for Chemical Analysis) (13) to determine the chemical compositions of their surfaces.

RESULTS AND DISCUSSION

Blown Film Extrusion

Extrusion conditions to produce films for physical testing were chosen such that LLDPE-1 (with 5% of the LLDPE-2 carrier resin) was melt fracture free when extruded from the wide die gap (2.3 mm). These conditions, listed in Table 2, were then held constant for production of film ",,,,,, ... ,,,1,,,.,, with both process These same were used when films were blown from the narrow die gap .0 mm). From this narrow gap, LLDPE-1, without PPA, exhibited melt fracture. No further attempts were made to improve conditions or the film

properties resulting from these initial settings. The frost line was maintained at a constant height of two die diameters throughout the study.

Similar criteria and considerations were used to select the extrusion conditions listed in Table 3 that were used to make films for surface analysis.

To magnify any potential effects, each of the processing additives was studied at a 1500 ppm level. This is in excess of typical use levels of 200-800 ppm. Previous work in this laboratory has shown a minimum level of 400 ppm of PPA-1 was required in LLDPE-1 to completely eliminate melt fracture in one hour, whereas 300 ppm of PPA-2 was equally effective in this same time period.

Extrusion Benefits.

In general, when the die gap was narrowed, pressure and amperage increased. This resulted in a rise in the melt temperature. Individual differences in melt temperature were more a function of the time of day as the extruder warmed. No attempts were made to compensate for this.

Table 2 shows a reduction in gate pressure of 6% and no change of amperage for the narrow die gap extrusion with PPA-1. PPA-2 provided a further pressure reduction of 12% at those conditions. Similar observations were made during the wide die gap extrusion. In some cases, the output decreased slightly with the improved process aid efficiency, extruder rpms were increased to maintain a constant film gauge. A normalization of extruder output to energy input shows PPA-2 to be the most output/energy efficient. This data is listed in Table 2.

Mechanical and Optical Properties.

Properties of films produced from the wide die gap are listed in Table 4. All properties listed, with the exception of dart impact, were unaffected by the addition of either process additive type. The individual values for tensile, tear, and optical properties for films produced with PPA-1 and PPA-2 were within the standard deviations for the melt fracture-free LLDPE-1 control film sample. The dart impact improved somewhat with addition of either PPA, indicating possible impact modification virtues for these products.

Although photomicrographs have shown the PPAs to be phase separated from the continuous polyethylene (10), their presence is very minor. Given that the fluoropolymer's density is approximately twice that of polyolefins, the additive's volume fraction is only half of its own weight fraction in LLDPE-1. Therefore, bulk effects, if any, should be insignificant.

Use of the narrower die gap increased the apparent shear rate in the die leading to melt fracture formation in LLDPE-1. It has been proposed that the presence of melt fracture can account for the decrease in certain properties measured for the control sample (14). Increasing the output would have increased the severity of the melt fracture, which eventually could have detracted from other properties.

Since all extrusions conditions were held constant when the die gap was constricted, and no attempt was made to optimize or capitalize on this change, many of the physical properties remained unchanged compared with samples from the wide gap. The narrowing of the gap did lead to a closer balance of transverse and machine direction tear values.

From the narrow gap, PPA-2 provided a noticeable reduction in percent haze and an improvement in gloss. Previous work in extrusion blowmolding has shown similar gloss improvements through the use of PPAs (15).

The advantages of narrower die gaps providing a thinner melt cross section and allowing for improvement in various film properties, gauge control, cooling, and output has been documented by many authors (16,17,18). In addition, improved cooling from a dual lip air ring can further improve optical and mechanical properties (16). The PPA's ability to reduce pressure, and to a lesser extent extruder amperage, can also allow for operation at lower melt temperatures. This can be advantageous for increasing output and decreasing degradation.

Of even greater potential, is the use of PPAs during resin design. From a polyethylene molecular architecture viewpoint, improvements in physical properties and processability tend to be at odds with each other. Rather than compromising between the two, the base polymer can be optimized for final physical properties, and PPA utilized for extrudability.

Heat Seal

Conditions of 0.5 seconds dwell, 1.5 bars of pressure, and two seal temperatures were used to generate the data listed in Table 4. For samples from the wide die gap, the average force to separate films remained unchanged with the addition of either PPA as compared with the control. There was no change in seal strength above or below the melt induction temperature.

From the narrow gap, both PPA containing samples were again within the test's margin of error. As expected, the melt fractured control sample exhibited lower seal strengths.

Surface Analysis

The film surface of samples both before and after corona treatment, and with and without each PPA, was analyzed the day of production, and one year later.

The surface energy of the films was assessed by several means as listed in Table 5. The surface energies for all the corona treated films were the same within experimental error. The surface energies of the untreated films were below the test solutions available, and thus not determined. Although the surface energies could not be measured, the work described below with ESCA, SSIMS, and contact angle showed no differences for these untreated samples.

The contact angles made by advancing and receding droplets of water were also measured. The ASTM wettability test is based on a receding phenomenon, where the test liquid is physically forced to wet the surface (advance) and its retraction (recession) is examined visually. This ASTM test is expected to correlate best to the receding water contact angle. Standard deviations for all angles measured were about 2°. The angles for films made with either PPA type, whether treated or not treated, and fabricated from the wide or narrow die gap, were all within the test error for the respective control specimens. This strongly suggests no differences in surfaces due to the presence of either PPA.

The higher recorded receding angles for the untreated films as compared with the corona treated films are indicative of their lower surface energy. The small hysteresis, or differential of advancing and receding angles, for the untreated films indicates a more homogeneous surface. This is confirmed by the elemental surface composition of the untreated films as determined by ESCA, and listed in Table 6. All untreated samples contain primarily carbon. The small amount of oxygen is probably due to oxidation and/or anti-oxidants present at the surface coming from the LLDPE base resins (19).

The elemental presence of either PPA type was not observed at the surface of the wide gap untreated films. Also, films from the narrower die gap, which were fabricated with increased shearing, did not show any evidence of process additive at \he surface. Fluorine is ene of the most detectable

by ESCA, which in these tests used a sampling area of 0.2 cm2. This is several orders of magnitude greater than the spacing of PPA particles. The surfaces of all the untreated films

remained virtually unchanged after one year of aging. This suggests no migration of any species from within the samples.

For the corona treated films, on the first day of testing, there was no difference in surface composition with either PPA in comparison to the control sample. There was also no dependance on the die gap, and hence shear rate, used to produce the films. After 12 months of aging, all six films were still similar. However, there was a uniform drop in elemental oxygen from the first day when it had been fixed to the surface by corona treatment. Others have reported this same observed drop in oxygen over time (20) and reported no change in adhesion despite it.

All film surfaces were also analyzed by SSIMS, which has greater surface sensitivity compared to ESCA. SSIMS is capable of detecting mono-layer thicknesses, and is more sensitive to lighter species. Fluorine ion would register as 19 amu's with a negative charge. Very low peaks at -19 were detected in the PPA samples, but they were also found in the non-PPA control samples. Given there was no detectable difference amongst the samples, a numerical analysis to identify the structure of these fragments was not performed.

Other Benefits.

The mechanism by which PPAs eliminate melt fracture and improve processing can also prevent the accumulation of low molecular weight polymer fractions, additives, pigments, etc within the extruder and die. This build-up can then degrade and/or cross-link and exit later as gels, black specks, etc. Production trials have confirmed this further benefit of reducing or eliminating die build-up in LOPE, LLOPE, HOPE, EVA copolymers and blends thereof. Production times between shutdowns can be greatly extended in cast film extrusion operations where melt temperatures are usually higher than in blown film.

Of all the properties, parameters, and materials analyzed, in no instance was the presence of elevated levels of either polymer processing additive (PPA) found to negatively effect or detract from those of the unmodified control samples. In several instances the presence of these products enhanced properties such as gloss and dart impact, and also reduced haze.

Given their innocuous and nearly inert physical presence, it may be more appropriate to consider these products as a production tool or process variable rather than as an additive. Indeed, their use permits the productioll of films beyolld the ex'rusion conditions previously limited by temperature, pressure, and melt fracture. Thus allowing even further improvements in productivity and final properties.

ACKNOWLEDGEMENTS

We would like to thank AT Plastics Inc. of Brampton, Ontario, Canada for the use of their blown film line and for measuring the mechanical and optical properties of the blown film samples.

REFERENCES

1. A. Rudin, A. Worm, and J. Blacklock, J. plast Film Sheet. "Fluorocarbon Elastomer Processing Aid in Film Extrusion of LLOPE's" 1(3): 189(1985)

"Th" Influenc€I oi Polyolefin AQ11::iIt"~9S on Aids" 1425( 1

3. B. Johnson, T. Blong, J. Kunde, and D. Duchesne, TAPPI 88 PLC Conf. "Factors Affecting the Interaction of Polyolefin Additives with Fluorocarbon Elastomer Polymer Processing Aids", 249(1988)

4. T. Blong, and D. Duchesne, SPE ANTEC 89 Goof Proc. "Effects of Antiblock! Processing Aid Combinations on LLDPE Blown Film Extrusion", 1336(1989)

5. D. Duchesne, H. Schreiber, B. Johnson, and T. Blong, SPE Ontario Section RETEC Proc. "New Approaches to the processing of Rutile-Filled Polyolefins", 1989

6. T. Blong, K. Fronek, B. Johnson, D. Klein, and J. Kunde, SPE polyolefins VII Int Conf. "Processing Additives and Acid Neutralizers-Formulation Options in Polyolefins", 1991

7. D. Priester and G. Chapman, SPE ANTEC 88 Conf Proc. "Fluoroelastomers in Polyolefin Film Production: An Economic Model", 1430( 1988)

8. M.C. Godin and C Gick, SPE ANTEC 85 Conf Proc. "LLDPE With Improved Processability", 454(1985)

9. 3M Method "AnalytiC Method for Determining Dynamar™ Concentration in Polyolefins"

1 O. 3M Method "Optical Microscopy Method for Dispersion Analysis in Polyolefins"

11. ASTM D-2578-67, ASTM Standards, Part 36 (1982)

1 2. D. Briggs, A. Brown, and J. Vickerman, Handbook of SSIMS, J. Wiley and sons, 1989

13. D. Briggs and M. Seah, practical Surface Analysis, 2nd Ed., J. Wiley and sons, 1990, Vol. 2.

14. V. Firdhaus and P.P. Tong, SPE ANTEC 92 Conf Proc. "Effect of Sharkskin Melt Fracture on LLDPE Properties", 2550(1992)

15. D. Duchesne, T.J. Blong, and M. Brandon, SPE ANTEC 93 Cont proc. "Processing Additives in High Density Polyethylene Extrusion Blow Moulding Applications", 2452(1993)

16. L.E. Dowd and M.L. Opacich, SPE ANTEC 85 Conf Proc. "Air Ring effects in Blown Film Extrusion", 40(1985)

1 7. B. Knittel, SPE ANTEC 84 Conf proc. "Improving Thickness and Shrinkage Uniformity of Blown Film Products", 23(1984)

18. W. Kurzbuch, J. plast. Film Sheet. "LLDPE Blown Film Productivity: Effects of Processing Temperature and Die Gap on Attainable Production Rates" 3: 125(1987)

19. F.C. Schwab and M.A. Kadash, J. Plast. Film Sheet. "Effect of Resin Additives on Corona Treatment of Polyethylene" 2: 119( 1986)

20. M.A. Mier and C. G. Seefried, SPE ANTEC 85 Conf Proc, "Surface Characterization of Corona Treated Polyethylene Films", 269(1985)

Table 1: Descriptions of LLDPE's

Resin LLDPE-1 LLDPE-2

Melt Index 1.0 2.0

Density (glee) 0.918 0.918

Co-Monomer 1-Hexene 1-Butene

Table 2: Production of Films from LLDPE-1 for Mechanical and Optical Property Testing

Sample Film line extrusion parameters at end of one hour 1500 Die gap Gate Pressure Melt Melt ppm mm kPa psi Amps kg / hr -A ° C Fracture - . - 2.3 25900 3760 129 0.67

PPA-1 2 .3 24940 3620 129 0.67 PPA-2 2 .3 23290 3380 11 7 0 .74

- - - 1.0 38310 5560 137 0.63 PPA- l 1.0 36030 5230 136 0.63 PPA-2 1.0 33620 4880 127 0.68

Extruder: 89 mm (3.5 in) Une speed: 25 mlmin 24 UD barrier screw Die Diameter: 20.3 cm 30-35 RPM Die Gaps: 2.3 mm

Output: 86 kg/hr (190 Ibs/hr) 1.0 mm Zones 1-5: 180°C (356 OF) Frost Line: 42 cm Adapter: 210°C (410 OF) Shear Rate: 55 s-l Die: 210°C (410 OF) 290 s-1

Table 3: Kiefel Film Line Extrusion Parameters, LLDPE-l Production of Films for Corona Treating and Surface Testing

Extruder: 40 mm (1.6 in) Die Diameter: 80 mm 24 UD grooved feed Die Gaps: 2.0 mm 90 RPM 0.6 mm

Output: 25 kg/hr (55 Ibslhr) Line speed: 15 mlmin Zones 1& 2: 210°C (410 OF) Gauge: 25 ~m Adapter: 220°C (428 OF) Frost Line: 20 cm Melt Temp: 205° C (401 OF) Shear Rate: 55 s-1 Die: 210 °C (410 OF) 610 5-1

206 None 208 None 211 None 225 100% 228 Removed 233 Removed

(82 ft/min) (8 in) BUR: 2/1 (90 mils) DDR: 30/1 (40 mils) DDR: 14/1 (16.5 in) (from 2.3 mm gap) (from 1.0 mm gap)

(3.1 in) BUR: 2/1 (79 mils) DDR: 40/1 (24 mils) DDR: 12/1 (50 ftlmin) (1 mil) (8 in) (from 2.0 mm die gap) (from 0.6 mm die gap)

Table 4: LLDPE-1 Physical Properties

2.3 mm Die Gap 1.0 mm Die Gap Control 1500 ppm Control 1500 ppm

Property NoPPA PPA-1 PPA -2 NoPPA PPA-1 PPA-2

Melt Fracture Nl Nl Nl Yes Nl Nl Average Gauge (microns) 35.9 36.7 36.3 38.8 36 .1 35 .2 Tensile (ASTM D-882)

Yield. Stress, MPa MD 12.64 12.61 12 .63 11 .23 12 .34 12 .56 TO 13.01 12.92 13.32 12.15 13.46 12.78

Yield % Elongation • TO 22 22 22 22 22 22 Break, S1ress, MPa MD 48 .88 47.17 48 .36 40.64 46.05 47.50

TO 37.32 36.59 38.19 35.26 42 .34 41 .04 Break % Elongation MD 631.5 622 .0 640 642 672 663

TO 741 .0 735.5 740 .0 721 758 .5 739 .5 Young's Modulus MPa MD 159.1 155.3 156.2 132.5 150.5 152 .5

TO 179.5 172.7 177 .9 157.4 184.2 165 .6 Elmendorf Tear crams MD 480 455 488 514 571 559

(ASTM D-1922) TO 975 978 996 740 860 828 Balance TD/MD 2.03 2.15 2 .04 1.44 1.51 1.48

Dart Impact grams F50 170 196 200 105 192 238 (ASTM D-1709 Method A) Seal Sirength 110 °C 1.58 1.57 1.67 1.34 1.46 1.46

average force, N 120 °C 11.18 11 .50 11.10 9.81 11 .24 10.73

% Transmission_, Gardner 93 .6 93 .6 93 .5 93 .6 93 .6 93 .5 % Haze 15 .9 18 .6 16 .2 14 .6 16 .9 9.5 % Gloss 45° Gardner 42.6 40.8 44 .7 45 .4 45.3 64 .9

Control: LLDPE-1 + 5% LLDPE-2 (to compensate for PPA concentrate carrier resin)

* % Yield MD: All samples yielded in the vicinity of 22%, but as there was no decrease in stress after yielding it was difficult to pinpoint the zero-slope plateau.

TO: Transverse Direction MD: Machine Direction

Table 5: Surface Wetting Analysis, Films from LLDPE-1

Sample Not Treated LLDPE-1 Day_one

+ 1500 Die gap sa ar

~ mm degrees

- - - 2.0 106 91 PPA- 1 2.0 107 91 PPA-2 2.0 107 91 - - • 0.6 108 90

PPA- l 0.6 107 90 PPA-2 0.6 107 91

* Melt fracture present

Water contact angles Sa: Advancing Contact Angle Sr: Receding Contact Angle

Corona Treated Day one

sa ar S. Energy degrees dynes/cm

69 25 48 70 26 48 70 27 46 72 24 48 70 26 48 69 24 48

ASTM: D 2578-67 Surface energy as dynes/cm Test error = 2 dynes/cm

Table 6: ESCA, Percent Elemental Composition of Films from LLDPE-1

Sample Not Treated Corona Treated LLDPE-1 da one 12 months day one 12 months

1500 I Die gap C a F C a F C 0 F C a p~ mm % % % % % % % % % % %

--- 2.0 99 .2 0.8 - 99.4 0.4 - 86.9 12.2 - 9 1.0 8 .6 PPA- 1 2.0 99. 6 0.4 - 98.9 0.6 - 88.4 11 .6 - 91. 5 8.5 PPA-2 2.0 99. 7 0.3 - 99.5 0.5 - 87.8 12.2 - 92.0 8.0 - - • 0.6 99.6 0.4 99.4 0.6 88.3 11.7 91 .3 8.7 - - -

PPA- l 0.6 99 .5 0.5 - 99.5 0.5 - 88 .4 1 i .6 - 90.9 9.1 PPA-2 0 .6 99 .5 0.5 - 99.3 0.7 - 88 .5 11.5 - 91 .2 8.5

* Melt fracture present

F %

------

Small amounts of Si «0.4%) were detected on several of the corona treated samples. It has been determined to be silicone lubricant from the corona treater.

The day one, corona treated, control sample from the 2.0 mm die gap exhibited about a percent of NItrogen, Ihis element can also be "fixed" to the surface by Corona discharge.

Presented at the 1993 TAPPI Polymer, Laminations, and Coatings Conference in Chicago, IL August 29-September 2,1993.

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