IMPROVED PERFORMANCE OF VIBRATION WELDED THERMOPLASTIC JOINTS

IMPROVED PERFORMANCE OF VIBRATION WELDED

THERMOPLASTIC JOINTS

CROSS REFERENCE TO RELATED APPLICATION

This application claims the benefit of U.S. provisional patent application number

60/006,334 filed November 8, 1996 which is incorporated herein by reference.

BACKGROUND OF THE INVENTION

The present invention relates to vibration welding or more particularly to vibration welding

of thermoplastic joints.

The ongoing demand to use thermoplastics to replace metals in automotive vehicle applications such as air induction systems has increased in recent years. It is estimated that by the year 2010, 21.4 million air intake manifold components will be produced using welding techniques. This invention concerns an improved method of vibration welding

thermoplastic joints, and the vibration welded articles produced by the method.

Vibration welding of thermoplastics such as nylon 6 and nylon 66 is well known in the

art. See V. K. Stokes, "Vibration Welding of Thermoplastics, Part I: Phenomenology ofthe Welding Process", Polymer Engineering and Science, 28, 718 (1988); V. K. Stokes, "Vibration Welding of Thermoplastics, Part II: Analysis ofthe Welding Process", Polymer Engineering and Science, 28, 728 (1988); V. K. Stokes, "Vibration Welding of Thermoplastics, Part III: Strength of Polycarbonate Butt Welds", Polymer Engineering and Science, 28, 989 (1988); V. K. Stokes, "Vibration Welding of Thermoplastics, Part IV: Strengths of Poly(Butylene Terephthalate), Polyetherimide, and Modified Polyphenyiene Oxide Butt Welds", Polymer Engineering and Science, 28, 998 (1988) and C. B. Bucknall,et al, "Hot Plate Welding of Plastics: Factors Affecting Weld Strength", Polymer Engineering and Science, 20, 432 (1980).

Vibration welding may be conducted by vibrating two parts under pressure along their common interface to generate frictional heat, and thereby melting and fusing their surfaces together. Vibration welding is a quick and inexpensive way to join irregularly shaped parts of various sizes. In the past, vibration welding has been used in low load-bearing applications. In automobile underhood applications such as air intake manifolds, air filter housings, and resonators, the expanded use of engineered plastics would be desirable to achieve savings and weight and cost. However, heretofore it has not been possible to achieve adequate weld strengths for such uses. Welding results are extremely sensitive to parameter uniformity and slight variations in them can result in significant changes in weld quality. Vibration welding parameters of pressure, frequency, amplitude, oscillation (welding) time, hold time and weld thickness all affect tensile strength of welds. It is an object ofthe present invention to provide a method for vibration welding fiber reinforced thermoplastic surfaces to provide welds having greater tensile strengths than have been heretofore achievable. U.S. patent 4,844,320 teaches that weld strength are not affected by weld amplitude or weld time above a certain level. In conventional vibration welding, welds are formed at a vibration amplitude of .03 to .70 inch. In contrast we have found that weld amplitude and weld time are extraordinarily important criteria for increasing weld strength. The vibration welding of this invention uses a vibration amplitude of at least about .075 inch. It has been determined that conventional vibration welds of reinforced thermoplastic surfaces achieve a maximum tensile strength of approximately

80% of a weld formed by the unreinforced surfaces of corresponding thermoplastic materials. For glass fiber reinforced thermoplastics, this lowered tensile strength is attributed to a change in the glass fiber orientation at the welded joint. According to this invention, vibration welds of reinforced thermoplastic surfaces achieve a maximum tensile strength of as high as about 120% of a weld formed by the unreinforced surfaces of corresponding thermoplastic materials. This is because fibers from at least one ofthe surfaces are caused to penetrate both into the weld and into the other surface. This provides added, unexpected tensile strength to the weld.

DESCRIPTION OF THE INVENTION The invention provides a method of attaching a first surface comprising a fiber reinforced first thermoplastic composition to a second surface comprising a second thermoplastic composition which method comprises contacting the first and second surfaces and vibration welding the contacted first and second surfaces under conditions sufficient to form a weld between the first and second surfaces which weld comprises a blend ofthe first and second thermoplastic compositions and wherein fibers from the first surface penetrate both into weld and the second surface. The invention also provides a vibration welded article which comprises a first surface comprising a fiber reinforced first thermoplastic composition, and a second surface comprising a second thermoplastic composition in contact with the first surface, and a

weld between the first and second surfaces comprising a blend ofthe first and second

thermoplastic compositions and wherein fibers from the first surface penetrate both into the weld and the second surface.

Techniques of vibration welding and apparatus for conducting vibration welding are well known in the art as exemplified by U.S. patent 4,844,320 which is incoφorated herein by reference. There are four phases to vibration welding of thermoplastics,

namely heating ofthe interface by friction; unsteady melting and flow of material in the lateral direction; melt zone establishment at a steady state condition; and unsteady flow and solidification ofthe materials at the weld zone upon cessation of vibration. Welding may be conducted by standard vibration welding equipment which have been

modified to achieve the parameter conditions required for the invention. The

parameters of significance include pressure, amplitude, frequency, weld cycle time and

hold time.

Vibration welders are commercially available from Branson Ultrasonics Coφoration,

Danbury, Connecticut, as a Mini- Vibration Welder and 90 series Vibration Welders model VW/6. However, these must be adjusted since their rated amplitude range is

.040 to .070 inches at 240 Hz output frequency. Vibration welding may be conducted

by placing a first thermoplastic surface and a second thermoplastic surface into contact under pressure. At least one and preferably both ofthe thermoplastic surfaces are fiber reinforced. The surfaces to be welded are placed into contact with one another and the interface between the surfaces is kept at a predetermined pressure, for example by positioning them on a platform under pressure applied by air or hydrauhc cylinders. Linear reciprocating motion is then imparted to one surface with respect to the other

surface to create a frictional rubbing which generates heat, melts the surfaces and blends the thermoplastic materials from the first and second surfaces. Prior to welding, the fibers in the fiber reinforced thermoplastic materials are substantially unoriented. In prior art vibration welding techniques, thermoplastic surfaces in contact melt and blend to form a weld, however, fibers positioned in the weld are only oriented within the plane ofthe weld. In contrast, when vibration welding is conducted according to this invention, fibers which reinforce the surface or surfaces are pressed into the opposite contacting surface. This achieves a heretofore unattainable weld strength

when the weld cools.

According to the invention, the two thermoplastic surfaces which may be welded are composed of any compatible thermoplastic polymeric material. Suitable thermoplastic polymers nonexclusively include polyamides, polyesters, polycarbonates, polysulfones, polyimides, polyurethanes, polyethers, vinyl polymers, and mixtures thereof. Polyamides such as nylon 6 and nylon 66, for example Capron * 8233 G HS nylon 6 and Capron* 5233G HS nylon 66 available from AlliedSignal Inc. of Morristown New Jersey and polyesters such as Petra* 130 polyethylene terephthalate available from AlliedSignal Inc. are most preferred. Dissimilar thermoplastic surface materials may be used provided they blend compatibly. At least one and preferably both ofthe thermoplastic surfaces are fiber reinforced. Suitable reinforcing fibers non-exclusively include materials which do not soften, i.e. lose their rigidity, at temperatures typically used for injection molding, such as temperatures of up to about 400 °C. Preferably the fiber reinforcement comprises such a material as glass, carbon, silicon, metals,

minerals, polymeric fibers and mixtures thereof. Glass fiber reinforcement is most preferred. In the preferred embodiment, the fiber is rigid and has a diameter of from

about 8 to about 12 micrometers, preferably from about 9 to about 11 micrometers

and most preferably about 10 micrometers. The preferred fiber length is from about 120 to about 300 micrometers, more preferably from about 130 to about 250 micrometers and most preferably from about 140 to about 200 micrometers. In the

preferred embodiment, the fibers comprises from about 6 to about 40 weight percent

ofthe thermoplastic composition, more preferably from about 13 to about 25 weight percent ofthe thermoplastic composition.

The linear peak-to-peak displacement or distance of rub of one surface on the other is the vibration amplitude. In the preferred embodiment, the vibration amplitude is at least about .075. More preferably the vibration amplitude ranges from about .075 to

about .15 inch and most preferably from about .075 to about .090 inch. The foregoing

amplitudes are at a nominal output vibration frequency of 240 Hz. At other vibration

frequencies the amplitude would vary. For example, at a nominal output vibration frequency of 120 Hz, the preferred vibration amplitude would range from at least

about .09 inch, more preferably from about .13 inch to about .16 inch and most

preferably from about .135 inch to about .145 inch. Vibration amplitudes for other frequencies can be easily determined by those skilled in the art. In the preferred embodiment, the contacting surfaces are held under a pressure, normal to the surfaces, of from about .6 to about 1.5 MPa during vibration welding. More preferably the pressure ranges from about .6 to about 1.2 MPa and most preferably from about .7 to about .8 MPa. The time of oscillation or rubbing time preferably ranges from about 2 to about 7 seconds, more preferably from about 4 to about 6 seconds. The hold time, or cooling time during which the pressure is maintained after stopping oscillations preferably ranges from about 2 to about 8 seconds, more preferably from about 4 to about 5 seconds. The weld thickness preferably ranges from about 160 to about 400 micrometers, more preferably from about 200 to about 350 micrometers and most preferably from about 250 to about 330 micrometers. When vibration welding is conducted under the foregoing conditions, a portion ofthe fibers from the reinforced surface penetrate into the weld and the opposite surface. When both surfaces comprise reinforced thermoplastics, a portion ofthe fibers from each surface penetrate both into the weld and the opposite surface. In the preferred embodiment, the estimated (by tensile strength) proportion of fibers from one or both reinforced surfaces penetrating into the opposite surface ranges from about 2 % to about 8 % preferably from about 4 % to about 8 %, and more preferably from about 5 % to about 8 %. As a result ofthe vibration welding process of this invention, welds of a reinforced thermoplastic surface to another thermoplastic surface achieve a higher maximum tensile compared to a weld formed by unreinforced surfaces of corresponding thermoplastic materials. The tensile strength of vibration welds of reinforced thermoplastic surfaces range from at least about 85 % and preferably from about 85 % to about 120% of a weld formed by the unreinforced surfaces of corresponding thermoplastic materials. Without being held to a particular theory, it is hypothesized that the vibration welding parameters of this invention allow fiber penetration from one reinforced surface into the other surface. For example, pressure application, and vibration time and amplitude should be conducive to pushing fibers from one melted surface into the other. Weld thickness which is too low or fiber loading which is too high may result in insufficient space for fiber rotation and hence restrain fiber crossing into the opposite surface.

The following non-limiting examples serve to illustrate the invention. It will be appreciated that variations in proportions and alternatives in elements ofthe components ofthe photosensitive coating composition will be apparent to those skilled in the art and are within the scope ofthe present invention.

EXAMPLE 1 Pellets of Capron* 8233G HS nylon 6 and Capron* 5233G HS nylon 66 available from AlliedSignal Inc. of Morristown New Jersey are injection molded into 3" x 4" x 1/4" and 3" x 4" x 1/8" blocks containing a nominal 0-50 weight % fiberglass reinforcement. Identical blocks are vibration welded together with a Mini- Vibration Welder or 2400 Series Welder from Branson Ultrasonics Coφoration using the following parameters: maximum clamp load: 4.5 kN; weld amplitude: .762 to 2.28 mm (0.030" to 0.090"); weld time: 4-8 seconds, nominal weld frequency: 240 Hz. Welding parameters, i.e. pressure (loading), amplitude and time were varied to optimize tensile strength ofthe welded joints. Only those samples which achieved a tensile strength higher than that ofthe base unfilled materials were selected to then study moφhology ofthe weld zones. Details ofthe zone interface and fiber orientation were included in

this analysis. Optical microscopy was used to study the moφhology ofthe samples, while image analysis was used to quantify fiber length.

Analysis of Glass Fibers Loading at Weld Zone

The nominal fiber loading ofthe Capron* nylon 6 injection molded parts that were studied ranged from 0 to 50 weight %. However, the actual fiber loading at the weld zone may vary if either fibers or the nylon matrix are preferably pushed away from the weld zone as the joint is formed. In order to determine whether the fiber loading in the excess flow region at the weld is different than in the bulk material, the weight % of fibers was measured by taking the weight difference ofthe excess before and after the matrix was pyrolized. The results of seven Capron* 8233 G HS nylon 6 samples processed under different welding conditions are summarized in Table 1. The results show that fiber loading ofthe various nylon 6 materials examined are approximately 0.5 wt.% to 1 wt.% lower than the bulk composition.

For nylon 66, the glass content in the weld zone flash was measured from Capron* 5233G HS nylon 66 samples. The results are given in Table 2 and show that fiber loading of nylon 66 at the weld zone flash are approximately 0.5 wt.% lower than the bulk composition. These fiber content variations are rather small and are close to the accuracy ofthe fiber content measurement.

Analysis of Glass Fiber Length at the Weld Zone

In order to determine whether there may be excessive breakage of fiber at the weld zone, an analysis of fiber length was conducted. Fiber length determination of fibers from the flash (recovered from pyrolysis ash) was measured by optical microscopy and by image analysis. Glass fiber samples were drawn from the ash and dispersed onto a glass slide with 2,2,2-trifluoroethanol (TFE) solvent. Ten optical micrographs were taken of each sample and a total of 1000-2000 fibers were digitized and measured by

the image analyzer. Table 3 summarizes the results. The analysis indicates that averaged fiber lengths of all samples are within the range of 120 to 180 micrometers. This is comparable to the fiber length average of samples measured from the original molded tensile bars away from the area ofthe weld zone. Furthermore, a study ofthe weld zone fracture surface by scanning electron microscopy suggested that there is no excessive breakage of fibers at the weld zone.

Analysis of Glass Fiber Orientation Distribution at the Weld Zone

The Fiber Orientation Distribution (FOD) of glass fibers (GF) at the weld zone was studied by optical and scanning electron microscopy. For each sample, both planar and through thickness sections were prepared and metallographically polished in preparation for optical microscopy study. Optical micrographs at relatively low magnifications (25x and 50x) show the general FOD around the weld zone as well as fiber orientation at the weld zone. Optical micrographs are taken from polished sections of nylon 6 samples with 6 wt.% GF, 14 wt.% GF, 25 wt.% GF, 33 wt.% GF and 50 wt.% GF, respectively. Micrographs show the fiber orientation both close to and away from the weld zone. Additionally the apparent thickness ofthe weld zone can be measured directly from the FOD changes with position shown in the micrograph. It is noted that for samples with 14 and 25 wt. % GF, there is apparent evidence of some fibers oriented in the tensile direction peφendicular to the weld plane. It was noted that the effects of reinforcement at optimized welding conditions appeared independent ofthe glass fiber orientation in the molded plaques which were selected for welded.

Tensile Strength of Weld Joints

For each vibration weld condition (i.e. a set pressure, amplitude and weld time), ten specimens were tested under the standard ASTM D638M-93 tensile testing procedure for plastics. Table 4 summarizes the results for weld joint tensile strength at optimized weld parameters. The influence of glass fiber loading on tensile strength is examined. These results indicate that all the weld joint samples have a tensile strength higher than that of unreinforced nylon 6. For the reinforced nylon 6 materials, the maximum tensile strength is 93.1 MPa. This occurs around 14 wt.% to 25 wt.% glass fiber loading. By comparison with the unreinforced material, which has a tensile strength of 79.3 MPa, this highest weld strength found in the reinforced grades represents a 17% increase in weld joint tensile strength.

The tensile strength of welded nylon 6 materials appears to be slightly higher (approx. 4%) than that of welded nylon 66 under the same welding and reinforcing conditions. The data also show that, at the interface, the glass fiber/nylon 66 composition is similar to that ofthe bulk composite. The observed higher weld strength ofthe glass filled nylon 6 at optimum welding process conditions may be attributed to several factors. For nylon 6, at some compositions and welding parameter choices, a percentage ofthe glass fibers appear to cross the weld plane at the interface. The width ofthe weld zone, which is around 200-300 micrometers, is comparable to the average length of

ll fibers. This may permit some mobility ofthe fiber to move in directions other than the primary resin flow direction during the weld, i.e., the fibers are not so confined to move along the flow direction as in a narrow weld zone. The weld zone thickness observed from the micrographs may be plotted as a function of fiber loading. It is noted that the weld zone thickness does go through a maximum at 14 wt.% fiber loading. This maximum occurs at the same location (14 wt.% to 25 wt.% glass fiber

(GF)) as does the tensile curve maximum. This further suggests that the thickness of weld zone has a positive influence on the tensile strength ofthe welded joint. By preparing weld specimens at different orientations to the predominant fiber orientation, studies of weld performance as a function ofthe glass fiber orientation distribution in the GF nylon 6 plaques were permitted. Results of this data suggest that at the welding interface the fiber orientation achieved in the region ofthe weld zone becomes independent ofthe predominant orientation of glass fiber in the bulk nylon 6, adjacent to the weld. This data for linear vibration welded polyamide butt joints shows an increase in tensile strength up to 35% in comparison with prior published data.

TABLE 1 Percentage of Glass Fiber in the Flash for Capron* 8233 G HS (nylon 6)

Sample No. Wt. % Fiber in the Flash

1 32.04

2 32.52

3 32.26

4 32.56

5 32.54

6 32.20

7 31.93

Average 32.29± 0.25

Capron* 8233G HS Bulk 33.01 ± 1.21

TABLE 2 Percentage of Glass Fiber in the Flash for Capron* 5233 G HS (nylon 66)

Sample ID wt % of Glass Fiber in wt.% of Glass Fiber in

Flash Bulk

5233 GHS 33.48 33.94

TABLE 3 Fiber Length Analysis for Capron* 8233G HS (nylon 6)

Sample ID No. of Fibers Averaged Length of Fiber (micrometers)

1 1775 124.7

2 1838 131.8

3 1106 151.9

4 1182 147.7

5 1018 167.8

6 1381 145.9

7 834 180.25

Capron* 8233G HS 1374 133.7

Bulk

TABLE 4

wt.% Glass Fiber Trade Name Tensile Strength, MPa

at Optimized Welding

Conditions

0 Capron* 8202 HS 79.3

6 Capron* 8230GHS 83.1

14 Capron* 8231 GHS 90.7

25 Capron* 8232GHS 90.2

33 Capron* 8233GHS 85.2

50 Capron* 8235GHS 80.5