3.2. Shrinkage Characteristics
The shrinkage behavior of the bonding-partners was evaluated at a pressure of 20 bar, 300 bar and 500 bar in the temperature range between the cross-over point (
Figure 3) to ambient temperature, shown in
Figure 4. Between the two bonding-partners, a clearly different shrinkage behavior can be observed. While PMMA exhibits only a slight decrease in specific volume at 5% due to its amorphous structure at 20 bar, the volume reduction for the semi-crystalline PP is clearly higher at about 17%. At higher pressures of 300 bar and 500 bar (used holding pressure level), the shrinkage of PP decreased to 14% (300 bar) and 13% (500 bar), respectively. Nevertheless, the shrinkage is still clearly higher than for PMMA, which shows only a marginal influence of the volume reduction by the increased pressure in the investigated area.
Due to the low pressure during the filling of the pin-like structures, as well as the cooling phase, shrinkage effects cannot be compensated to a sufficient extent in the pin-like joining using the vibratory welding process. The clearly greater decrease in specific volume for PP (almost 3.5 times higher as PMMA) leads to the expectation of greater shrinkage effects and thus possibly larger hollows or gaps in the pin area for the material combination PA66-PP, compared to PA66-PMMA. At pressures of 300 bar and 500 bar, shrinkage effects still occur during the cooling phase of the injection molding process. However, it can be expected that these effects will be compensated to a certain degree by the holding pressure, and thus an increased structural filling will be achieved.
3.3. Filling Behavior
The optical evaluation of the filling behavior of the pin-like structures is shown in
Figure 5,
Figure 6,
Figure 7,
Figure 8 and
Figure 9.
Table 2 gives the analyzed unfilled areas in percentage of the form-fit connection for all process variants. There are only minor differences between the evaluation methods. On the one hand, these differences are due to the approximation of the unfilled areas at the invisible pin flanks and the analysis of only one sectional plane for the two-dimensional CT images. On the other hand, gray level variations in the transition areas of both materials may also slightly influence the three-dimensional MAVI evaluation. Due to the very similar results and identical trends, further discussion will be based on the two-dimensional analysis of the CT images, as results were generated for all variants here.
In the conventional joining step using vibration welding technology without pre-heating of the structured-partner (
Figure 5), an almost complete structure filling is shown for the bonding-partner PMMA. Unfilled areas are only visible in the pin-foot area (gap of approximately 10–20 µm and air inclusions in the edge areas) and slightly on the lateral pin surface. The evaluation of the structure filling (
Table 2) shows a filling of approximately 93% of the generated pin cavity (unfilled area: 7.2%). In comparison, the multi-material bond with PP as the bonding partner clearly shows that more unfilled areas (13.1%), as well as a structure filling of approximately 87%, are achieved. The unfilled areas are located on the lateral pin surfaces and in particular in the lower pin foot area. Here, a gap of about 60 µm is visible.
The results show that the filling behavior is clearly dependent on the bonding-partner. For both variants, PP and PMMA, a non-complete filling can be assumed during the joining step, as can be seen by the rounded edge areas of the flow front. The degree of filling achieved is significantly higher for PMMA. This is attributable to lower shrinkage effects as well as to the temperature range in which flow can take place. This temperature range is very small for PP, between approximately 174 °C (joining temperature [
16]) and about 168 °C (
Figure 3), whereas for PMMA, flow can occur between approximately 228 °C (joining temperature [
16]) and 190 °C (
Figure 3). A difference in the structure filling caused by the flowability of the bonding-partner is not to be expected for the two selected materials. PP and PMMA have a similar viscosity level in the flow range, whereby the complex viscosity for PP is even at a slightly lower level (PP: approximately 400–500 Pa s, PMMA: approximately 600–1000 Pa s [
16]).
The achievable cavity filling when the structured-partner is pre-heated to 80 °C or 120 °C during the joining step is shown for PMMA in
Figure 6 and PP in
Figure 7. For the bonding-partner PMMA, an improved filling of the structure is visible, especially for the higher pre-heating temperature. The air inclusions in the edge areas of the pin foot could be reduced and a filling of 97.4% was achieved at a pre-heating temperature of 120 °C (93.6% for pre-heating temperature of 80 °C). In contrast, a surrounding gap can be seen for the bonding-partner PP even when the structured-partner is pre-heated. With a thickness of 50–55 µm, the gap in the pin foot area is smaller than for the multi-material bond without pre-heating. The pre-heating slightly increases the degree of filling to 87.8% (80 °C pre-heating) and 90.9% (120 °C pre-heating). Striking is the shape of the cavity filling in the lower pin area. While the PP flow front is rounded without pre-heating of the structured-partner, these corner areas have sharp edges when the PA66 is pre-heated, independent of the pre-heating temperature. Further, the PP flow front reproduces the surface structure of the PA66 more accurately with pre-heating. The changed flow front in combination with the clear reproduction of the PA66 surface structure indicates a complete structure filling during the joining step with subsequent shrinkage. The improved filling can be explained by a reduced cooling rate during the filling of the cavity. Cooling of the melt formed in the joining zone begins directly as it flows into the cavity area. Due to the lower temperature difference caused by the pre-heated structured-partner, the melt cools slower and thus remains flowable for a longer time. During solidification and cooling, shrinkage effects result that cannot be compensated for due to the low pressure level in the vibration welding process and a missing melt layer. As a result, the volume of the PP decreases, resulting in a clearly visible gap between the two materials.
Compared to the pvT model, the unfilled volume of the multi-material joint is in the range of the evaluated volume shrinkage of the bonding-partner. The clearly increased shrinkage of the semi-crystalline PP (compared to PMMA) in the pvT is also evident for the form-fit joint. The slightly lower values for the multi-material connection with pre-heated structured-partner (here complete filling of the cavity during joining can be assumed) compared to the pvT can be explained by the simplifications made. The pressure present in the cavity area between the pin-like structures can be higher than the assumed pressure of 20 bar. This pressure is effective in the joining zone, referred to the total contact area of the two partners. Due to the reduced cavity area, where melt flow takes place, a higher pressure can exist locally. Furthermore, the cross-over point was determined in a rotational viscometer at low shear. The effective shear stress in the pin area may be increased, which would lead to a shift of the flow area to lower temperatures. Both would result in a reduction in shrinkage. Finally, during cooling of the pre-heated structured-partner, a change in length takes place due to the existing thermal expansion. This slightly reduces the volume of the cavity area compared to the filling process, which in turn results also in reduced shrinkage effects. Nevertheless, the trends evaluated are in agreement, regardless of the simplifications made.
The optical characterization of the multi-material bond produced by assembly injection molding is shown for the bonding-partner PMMA in
Figure 8 and for PP in
Figure 9. For both bonding-partners, the result is an almost complete filling of the cavity. The holding pressure level shows no significant influence in the investigated area. For all variants, a filling degree of approximately 93–96% (
Table 2) is achieved and the negative structure of PA66 is exactly reproduced by the bonding-partner. Despite the clearly different volume shrinkage of the two bonding-partners (
Figure 4), the filling levels is in a similar range. Shrinkage effects can be compensated in a wide range by the higher pressure during cooling in the injection molding process, as comparisons with the pvT measurement at 300 bar and 500 bar show, especially for the semi-crystalline PP.
For all variants, a surrounding, small gap can be seen between the two materials.
In contrast to the joints produced in the vibration welding process, a gap is also visible in the area of the PA66 pin head in injection molding. Due to the clear reproduction accuracy of the surface structure of the PA66 in all areas, complete filling in the joining step and subsequent shrinkage during cooling can be assumed. In areas with a sharp undercut, the gap is smaller than in areas without vertical undercut. The undercut structures prevent shrinkage of the bonding partner due to mechanical interlocks, whereas on free surfaces a clearly lower resistance to volume shrinkage is present. At the PA66 pin head area, unhindered shrinkage takes place. Thermal expansion effects during cooling of the PA66 component from mold to ambient temperature can also have a slight influence on the resulting gaps. The clear difference in the PA66 pin head area between the two joining methods (injection molding or vibration welding) can be attributed to the aggregate condition of the bonding-partner during the joining step. While in the vibration welding process the bonding-partner is in solid form and is only plasticized in the contact zone with the structured-partner, in the injection molding process the bonding-partner is completely molten and solidifies after the pin-like structure has been filled. Due to this increased melt volume in the pin head area, shrinkage effects are much more pronounced at this area. However, this presumably affects the mechanical properties of the multi-material connection only negligibly, since there are no undercuts in the area with increased shrinkage and thus the form-fit connection is not limited.
In addition to the rheological material properties, investigations show that shrinkage effects mainly influence the filling degree. Especially for bonding-partners with high shrinkage, these cannot be compensated for in the conventional joining step using vibration welding technology (with as well as without pre-heating) due to the low pressure level. Here, comparatively wide, unfilled areas result, which presumably will affect the bond properties as well.
3.4. Bond Properties
The mechanical bond properties of the multi-material joints produced by vibration welding technology without pre-heating and by assembly injection molding are shown in
Figure 10. Regardless of the manufacturing process, the PA66-PMMA joint exhibits a bond force in the range of 2000 N. For the PA66-PP combination, a clear difference can be seen depending on the joining step. While joints produced by assembly injection molding, irrespective of the holding pressure level, exhibit bond forces in the range of 1200–1300 N, the bond force for joints produced by vibration welding is significantly lower, at approximately 500 N. This can be attributed to the degree of filling of the structures achieved in the joining step. While for PMMA as a bonding-partner, similar filling degrees and, in particular, also a filling of the pin-foot area, can be achieved for both joining variants, for PP a clearly reduced filling takes place using vibration welding technology. Especially along the pin sides and in the bottom edge areas of the pins, unfilled areas remain for the PA66-PP combination. These reduce the resulting undercut area, which means that the theoretical form fit can only be partially utilized. The fracture behavior of the multi-material joint based on pin-like structures also clearly shows the influence of filling behavior. For joints between PA66 and PMMA (high degree of filling for all variants), cohesive failure by fracture takes place throughout. The fracture occurs for injection-molded joints always and for vibration-welded joints predominantly at the pin-foot area of the PMMA components. In contrast, the PA66-PP joint shows adhesive failure by pull-out of the PP from the pin gaps of the PA66 when vibration welding technique was used. For the increased degrees of filling (similar to those of the PA66-PMMA joints) achieved by injection molding, a predominantly cohesive failure occurs due to fracture of the PP component in the pin-foot area. The material strength can thus be fully utilized for the underlying pin geometry due to the increased filling behavior.
The mechanical characterization thus agrees well with the optical analysis of the filling behavior. In general, it can be stated that for high-shrinkage bonding-partners (usually semi-crystalline thermoplastics), filling and cooling under increased pressure has advantages with regard to the degree of filling and, as a result, to the bond quality. For bonding-partners with low shrinkage (e.g., amorphous thermoplastics), the pressure during the filling process is negligible for the bond quality as soon as a complete filling of the structure is achieved.