5.1. DMEAV Phases
Phase 1—Define: Project charter, working team, the related information, and study objectives were defined. The team members become familiar with the defined problem, the equipment used for 3D printing, the FDM printing method, the material of filaments used, the testing and measurement equipment and process, and the final product. The shape of the sample according to ISO 527-2:2012 [
45] and the face shield frame (STL file) are shown in
Figure 2.
The influence of process parameters on the quality of the result must be studied to understand the performance and behavior of the FDM process [
46]. The team received information that the printing process, tensile test, and dimension measurement will be performed in Neksten, s.r.o. Košice laboratories by laboratory engineer and operator, in the room with a constant temperature of 21 °C and humidity of 35%. The PLA, PETG, and PHA samples will be created with the 3D printer Original Prusa I3 MK3S+. Tensile tests will be performed according to the ISO 527-1:2019 [
47] standardized procedure using the testing machine Tinius Olsen H10KS (Tinus Olsen, Horsham, PA, USA), dimensional measurements using a caliper CD-15DCX with measuring range 0–150 mm, accuracy ± 0.02 (Mitutoyo Corporation, mensional measurements using a caliper CD-15DCX, Japan), and energy consumption meter Geti GPM01 (Geti, Sobrance, Slovakia).
Phase 2—Measure: For this phase, the team identified process responses and factors. Initially, at the recommendation of the Mondragon University AM Lab, printer manufacturer, filament supplier, literature search, and previous team experience, 17 factors (
Table S1) were identified that affect the resulting characteristics of the 3D product. Finally, five controllable factors were included in this research. The definitions of the controllable factors selected in this study are as follows:
Layer thickness/height [mm]: The nominal layer thickness for most machines is around 0.1 mm; however, it should be noted that this is only a general principle. The reasoning is that thicker layer parts are quicker to build but are less precise.
A number of perimeters: Defines the minimum number of outlines that form the wall of a printed product. According to [
23], product strength is defined mainly by the number of perimeters.
Extrusion width [mm]: It is a process used to create fixed cross-sectional profile objects. The filament is pushed through a die of the desired cross-section.
Infill density [%]: Infill provides internal support for top layers, which would otherwise have to bridge over the empty space. Most products can be printed with 10-15% infill [
48].
Nozzle temperature [°C]: Temperature for melting filament. Each material has a recommended temperature.
The output responses that will be measured were also defined:
Carbon dioxide equivalent (CO
2-eq) is the standardized measure for calculating the amount of greenhouse gases (GHG) emitted into the atmosphere due to a process or material use. This evolves into the Global Warming Potential (GWP) impact category, one of the main metrics used when assessing the potential impact of anything analyzed [
50].
Phase 3—Experiment: Five controllable factors and two levels for each factor (
Table 1) were defined in the previous phase. Regarding the setting of other factors, some are uncontrollable, others were set according to the manufacturer’s recommendations, and the remaining two factors are set according to
Table 2. The fractional factorial design (2
5−1) of resolution “V”, which is 1/2 fraction, was selected with design generator E = ABCD. This design allows for the analysis of the main effects and the interactions of the second order. Minitab 19 software (Minitab LLC, State College, PA, USA) created the experimental plan.
For the first experiment total of 96 samples (16 × 2 replicates × 3 materials), and for the second experiment total of 48 samples (16 × 1 replicate × 3 materials) were printed.
Regarding the selection of gyroid infill pattern, the final product (face shield) was taken into account, which is printed almost without the infill, and its pattern was in the first printing instructions. The face shield is thin, and its strength and flexibility depend more on the used material and the number of perimeters. Furthermore, according to [
51], the Gyroid is Prusa printers’ favorite and one of the best infills, provides outstanding support in every direction, is printed relatively fast, saves material, and does not have crossing lines in one layer.
Measured output responses for the first experiment are mechanical properties (young modulus, tensile stress at break, elongation), accuracy (thickness, width, length), weight, printing time, and material price (
Tables S2–S4). Responses for the second experiment are weight, printing time, filament price, and carbon dioxide equivalent (
Tables S5–S7). Detail of the sample surface was imaged by a scanning electron microscope (SEM) JSM-IT700HR (JEOL, Tokyo, Japan).
The sample images and the tensile test graphs are in
Figure 3,
Figure 4 and
Figure 5 for PLA Galaxy Silver, PETG Orange PPE, and PHA BioWOOD Rosa, respectively. Stress–strain curves in the graphs are for different experimental settings. The figure shows the extent to which the printer settings can affect the mechanical properties of products made of the same material. The tensile test stops when the sample breaks.
Fibrous, fiber-like protrusions were observed on the surface of the specimens made of Prusament PLA Galaxy Silver, which can be explained by the material’s viscid, less viscous but sticky nature. The tensile stress at break and elongation varies from 22.5 MPa to 52.2 MPa and from 122% to 314%, respectively.
A flow pattern with a rounded end can be seen on the surface of the specimens made of PETG Orange PPE. The openings in the surface resulting from printing were irregular in shape, which may indicate rapid solidification. No foreign particles were detected. The tensile stress at break and elongation varies from 22.3 MPa to 43.8 MPa and from 132% to 332%, respectively.
In the case of plastics containing biomass particles (PHA BioWOOD Rosa), the particles can be seen even at low magnifications, their distribution is even, and they have several sizes. The plastic does not form a bond, and a gap is formed around the particles. Many small elliptical openings, which sometimes have jagged edges, are on the surface. The tensile stress at break and elongation varies from 10.8 MPa to 21.8 MPa and from 116% to 191%, respectively.
Phase 4—Analyze: According to the procedure in
Figure 1, the obtained data are analyzed and optimized for each experiment separately. The first experiment analyzes mechanical properties and dimensional accuracy, and the second experiment analyzes environmental sustainability. Coefficients of the polynomial model were defined according to formula (1), and then analysis of variance (ANOVA), normal probability plot (NPP), main effect plot, and interaction plot were created for each response.
The
p-value less than 0.05 in ANOVA means that the factor is statistically significant. In the NPP diagram, the main and interaction effects of the factors are plotted against the cumulative probability. Inactive main and interaction effects tend to fall roughly along a straight line, whereas active effects appear as extreme points falling off each end of the straight line [
52]. These active effects are evaluated to be statistically significant. The main effect plot shows the mean response values at each design parameter or process variable level. It is used to compare the relative strength of the effects of various factors. The last interactions plot displays the mean response of two factors at all possible combinations of their settings. Horizontal lines indicate that there is no interaction between the factors.
Minitab 19 software was used for both analyses, which are based on calculating the effects of each factor. Graphical presentation of analysis results of selected responses (young modulus and length accuracy, PLA material) for the first experimentation with 32 samples is in
Figure 6. Other figures for PETG and PHA materials are in
Figures S1–S4.
The
p-values of factors and interactions are listed in analysis of variance. Statistically significant factors and interactions at the significance level α = 0.05 are marked in red on the normal plot. The first normal plot for the Young modulus in
Figure 6 does not contain statistically significant factors. The second normal plot for length accuracy in
Figure 7 shows significant factor A—layer thickness, BD—number of perimeters*infill density, and CE—extrusion width*nozzle temperature. The main effects plot has non-horizontal lines through the X-axis for factors that are important for the response. The non-parallel lines on the interaction plot indicate the relationship between the factors. Polynomial models in
Figure 6 and
Figure 7 are in un-coded units and should be reduced by omitting factors and interactions with low influence.
Table 3 summarizes the result of the analysis. It contains statistically significant factors and interactions where the
p-value is less than 0.05.
Table 4 lists measured dimensional accuracy of samples printed with various setups for all three materials. The table contains absolute deviations from the nominal dimensions of the sample. The lowest overall range (marked in green) was measured for PETG and the highest (red) for PHA material.
The analysis of the first experimental data reveals that there is no clear answer for the question of which factors are most significant for all three materials. For each material, other factors are significant. There were results such as PLA young modulus that do not have any significant factors. On the other hand, there were many significant factors and interactions for PETG. These results show that each material will require an individual approach when setting the print parameters and the manufacturer’s recommendation for a given filament is not sufficient.
After the first results were obtained, the second batch of 16 samples had been printed out. Geti GPM01 measured the consumed electrical energy for each sample. The LCA GaBi software (Sphera Solution, Leinfelden-Echterdingen, Germany) and the Ecoinvent 3.7 database (iPoint-systems, Reutlingen, Germany) were used for conversion of the energy [kWh] to CO
2-eq [kg]. The electricity mix of Slovakia and ReCiPe method as a model for environmental impacts assessment [
53] has been used. The values of the CO
2-eq correspond only to the 3D-printing process. Results of the second analysis for PLA material are presented in
Figure 8. Other figures for PETG and PHA materials are in
Figures S5 and S6.
The normal plot in
Figure 7 shows that the most important factors are A—layer thickness and B—number of perimeters. The main effect plot for sustainability has three non-horizontal lines through the X-axis, which are essential for the response, and include A—layer thickness, B—number of perimeters, C—extrusion width. On the interaction plot graphs, the lines are not parallel. The interaction plot indicates the relationship between DE—infill density*nozzle temperature.
Table 5 summarizes the result of the analysis for all three materials.
The factor A—layer thickness is significant for all three materials. This is obvious because a thinner layer means longer printing times and higher power consumption. Factor B—number of perimeters is significant only for PLA, but factors C—extrusion width and D—infill density are significant for two materials (PETG and PHA). From the main effect plot it can be seen that the layer thickness has the highest slope being the factor with the greatest effect for all materials. The infill density and extrusion width are the second most influential for PETG and PHA. Infill density makes the printing more environmentally sustainable when it is smaller. Interestingly, in this case, the nozzle temperature does not significantly affect sustainability, although a higher temperature would appear to cause higher energy consumption.
Once the analysis has been carried out and the significance of each factor is known, the optimal level of variables was found, according to various optimization objectives in
Section 5.2.
5.2. Optimization
Minitab 19 software uses the term individual desirability (d) for single-objective optimization and composite desirability (D) for multi-objective optimization to define the optimization objective. The desirability has a range of zero to one. Composite desirability is a weighted average of individual desirabilities.
The optimization objective for the first experiment is the composite desirability for all responses (young modulus; tensile stress at break; elongation; weight; width, thickness and length accuracy; printing time; and power consumption). All responses have the same weight value. Optimal levels of factors for each material are summarized in
Table 6.
Figure S7 shows the values of composite desirability and individual desirabilities for all responses.
The optimization objective for the second experiment is the composite desirability consisting of sustainability and filament price.
Figure 9 shows the value of composite desirability, individual desirabilities, and optimal values in red color for PHA material. Values for the remaining materials are presented in
Figure S8, and optimal levels of factors for all materials are summarized in
Table 7. The effect of nozzle temperature on the desirability value is small. Therefore, it is possible to set this factor to another value that will improve other properties, such as young modulus or length accuracy.
Phase 5—Verify: The team validated that the final 3D printer setup for printing face shield frames is effective and environmentally sustainable. For verification, we printed a batch of 30 frames (
Figure 10a) from PHA material according to Prusa Research design in
Figure 2b. The printer used the optimal setup in
Table 7, and the material selection is explained in
Section 5.3. Measurement System Analysis (MSA) calculated by Minitab 19 shows that the measurement system’s Total Variance (TV) is less than 10%. Measurement of the thirty printed face shield frames (
Figure 10a) showed that the distance between fasting pins a+b+c (
Figure 10b) was in the range (−0.3, +0.3) mm, which allowed the connection with the counterpart without problem (
Figure 10c).
Process capability index is one of the ways to assess the 3D-printing process performance. From the process capability index, it is possible to determine the number of non-conforming products, the production of which unnecessarily burdens the environment. This phase is not finished because measurements are not available yet.