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Article

Exploring Anisotropic Mechanical Characteristics in 3D-Printed Polymer Biocomposites Filled with Waste Vegetal Fibers

by
Honggang Wang
1,2,
Zhi Fu
2,
Yu Liu
2,
Ping Cheng
1,3,*,
Kui Wang
1,* and
Yong Peng
1
1
School of Traffic & Transportation Engineering, Central South University, Changsha 410075, China
2
China Automotive Engineering Research Institute Co., Ltd., Chongqing 401122, China
3
Laboratory of Engineering, Computer Science and Imagery (ICUBE), Centre National de la Recherche Scientifique (CNRS), University of Strasbourg, 67000 Strasbourg, France
*
Authors to whom correspondence should be addressed.
Symmetry 2024, 16(1), 70; https://doi.org/10.3390/sym16010070
Submission received: 26 November 2023 / Revised: 2 January 2024 / Accepted: 3 January 2024 / Published: 4 January 2024
(This article belongs to the Special Issue Advances in Composite Materials and Structures: Processing, Properties and Applications)
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Abstract

:
The fiber-filled polymer composite is one of the best materials which provides a symmetrical superior strength and stiffness to structures. With the strengthening of people’s environmental protection and resource reuse consciousness, the development of renewable materials, especially natural fiber-filled polymer composites, is receiving great attention. This study investigated the mechanical properties of polymer composites incorporating waste materials from the food processing industry and agricultural sources. Waste vegetal fiber-filled polymer biocomposites (WVFFPBs) with varying fiber types and 3D printing orientations were systematically fabricated. Subsequently, the tensile tests were executed to comprehensively assess the anisotropic mechanical behaviors of the WVFFPBs. The results demonstrated that WVFFPBs performed excellent anisotropic mechanical properties compared to pristine matrix samples as print orientation changed. As the printing angle increased from 0° to 90°, the tensile mechanical properties of the WVFFPBs displayed a decreasing trend. Moreover, the print orientation–anisotropic mechanical behavior relationship of 3D-printed WVFFPBs was revealed through the analysis of the material manufacturing characteristics and damage features.

1. Introduction

3D printing, also known as additive manufacturing (AM), has gained extensive popularity for its ability to swiftly produce intricate polymer components [1,2,3]. Among the various AM techniques for polymer-based fabrication, fused filament fabrication (FFF) has emerged as a prevalent method, primarily attributable to its cost-effectiveness and user-friendly operation [4,5]. Nevertheless, the inherent mechanical limitations of pristine polymer parts produced via FFF hinder their broader utility [6,7]. Thus, the short fibers are increasingly used as reinforcements introduced into FFF processing to improve the mechanical properties of FFF-printed components [8,9].
In recent years, the 3D printing of short fiber-filled composites has received more and more attention [10,11,12]. Jiang et al. [9] enhanced the mechanical properties of plastic FFF parts by adding short carbon fibers to the thermoplastic polymer filament to form a carbon fiber-filled polymer composite. Ma et al. [13] studied the relationship between the short carbon fiber content and mechanical properties; when the fiber content was 3 wt%, the flexural strength and compressive strength of the composites were 309.2% and 375.8% higher than those of nonreinforced samples, respectively. Billah et al. [14] investigated pristine and composite Acrylonitrile Butadiene Styrene (ABS) filled with short carbon and glass fibers using thermophysical and thermomechanical characterization techniques. The results showed that short fiber-filled composites possessed better thermomechanical properties. In the existing literature, they focused on the 3D printing process and mechanical properties of synthetic fiber-filled composites [15]. However, in light of the escalating environmental challenges confronting the global ecosystem, composites fortified with synthetic fiber reinforcements no longer align with the contemporary imperatives of environmental sustainability and eco-friendly development [16,17].
Natural fibers are gaining momentum as reinforcements for polymer matrix composite due to their biodegradable properties [18]. Furthermore, their availability, non-toxicity, lightweight, low cost, high specific stiffness, recyclability, and economic viability draw greater attention from researchers [19,20,21]. Tao et al. [22] investigated the compression property of 3D-printed short wood fiber-filled composite cellular structures using finite element simulations and compression experiments. Balla et al. [23] used soybean hull-derived fibers as reinforcements to manufacture thermoplastic copolyester composites by the FFF 3D printing process. The results showed that there was a strong dependence of surface quality and interface bonding on the short fiber treatment. Le Duigou et al. [24] studied the hygroscopic properties of wood fiber-filled composites and proposed that FFF of hygromorphic biocomposites enabled a shift toward 4D printing since the material was able to evolve over time in response to an external stimulus. According to the above research, the addition of vegetal fibers could bring good mechanical property and functionality to 3D-printed samples. More importantly, vegetal short fibers provide better anisotropic mechanical properties.
Therefore, in this work, the waste vegetal fiber-filled polymer biocomposites (WVFFPBs) with different fiber types were fabricated in different print orientations. The tensile test was performed to obtain the mechanical properties of the WVFFPBs. The anisotropic mechanical behaviors of WVFFPBs and pristine PLA matrix samples manufactured in different print orientations were compared. Furthermore, the failure features of the 3D-printed WVFFPBs were analyzed to reveal the print orientation–anisotropic mechanical behavior relationship.

2. Experimental Method

2.1. Materials and Processing

This work considered six different filament materials with a diameter of 1.75 mm: polylactic acid (PLA), short tomato, pruned orange tree, and hemp and weed vegetal fiber-filled PLA filaments. The PLA filament was purchased from eSUN (Shenzhen, China), and the short vegetal fiber-filled PLA filaments were acquired from Kanèsis (Puglia, Italy). The all short vegetal fiber dimensions were around 300 microns according to the information provided by the filament supplier. The vegetal fibers were 100% produced from agricultural by-products and surplus, no longer considered as “waste”. In detail, these waste short fibers were taken from Italian tomatoes (tomato), pruned orange trees (pruned), hemp shives (hemp), and hemp buds (weed). The information about the filaments is summarized in Table 1. Prior to use, each filament was stored in the filament storage box with a drying effect.
A commercial 3D printer, Raise3D (N2 Plus, Costa Mesa, CA, USA), based on the FFF technique was applied to fabricate the samples. During the printing process, the filament was fed into the nozzle and extruded on the printing bed, as shown in Figure 1a. According to the suggestion of the filament suppliers, the printing parameters for PLA were set to a layer thickness of 0.2 mm, a printing speed of 30 mm/s, and a nozzle temperature of 200 °C; the printing parameters for short vegetal fiber-filled PLA filaments were set to a layer thickness of 0.2 mm, a printing speed of 30 mm/s, and a nozzle temperature of 185 °C. The print orientation of samples is illustrated in Figure 1b; the samples with different print orientations were prepared to investigate the anisotropic mechanical properties of PLA and WVFFPBs.

2.2. Characterization

Thermogravimetric analysis (TGA) was performed using a Mettler TGA/DSC 3+ simultaneous thermal analyzer (Mettler Toledo Co., Zurich, Switzerland). Samples with a mass of 6.8 ± 2.1 mg were cut from the raw filaments. The materials were heated from room temperature to 800 °C at a heating rate of 10 °C/min in a pure nitrogen atmosphere [25,26]. Field emission scanning electron microscopy (FE-SEM, Hitachi Co., S-4800, Tokyo, Japan) was used to characterize the morphological behaviors of the vegetal fiber-filled filaments. The fracture morphological features of the samples were observed by a stereoscope (AO-3M150GS, AOSVI, Shenzhen, China).
The tensile properties of the samples were evaluated using a universal mechanical testing machine (E44, MTS Co., Eden Prairie, MN, USA) with a cross-head displacement speed of 1 mm/min. According to the standard of ASTM D638-10 [27], the tensile test sample with a length of 115 mm, a thickness of 3.2 mm, and a width of 6 mm was prepared. The tensile strength was taken as the breakage strength of the materials; the elongation at break was calculated by dividing the fracture displacement by the length of the sample. Each measurement was averaged from the results of five repeated tests.

3. Results and Discussions

3.1. Thermal and Morphological Behaviors of the Filaments

In this work, scanning electron microscopy (SEM) was used to investigate the cryofracture morphology of pristine PLA and the short tomato and hemp vegetal fiber-filled PLA filaments. The cross-sectional images of the WVFFPB 3D printing filaments with a diameter of 1.75 mm are shown in Figure 2a,e. There were a large number of unevenly distributed pores in the filaments, as shown in Figure 2. The diameter of the pores in the tomato and hemp fiber-filled PLA filaments were similar, as shown in Figure 2c,g. The appearance of pores could be attributed to the addition of short vegetal fibers that generated a large amount of gas during the filament manufacturing process. As shown in Figure 2c,d,g,h, the tomato and hemp fiber-filled PLA filaments were observed at higher magnification to further analyze the characteristics of the filaments. The shape of the pore was approximately circular, with fewer short fibers in the filaments, and only a small amount of fibers could be observed in Figure 2.
The tensile properties of short vegetal fiber-filled filaments are shown in Figure 3a; the hemp fiber-filled PLA filament exhibited the highest tensile strength (29.69 MPa), which was 11.74% higher than the tomato fiber-filled PLA filament (minimum tensile strength). TGA curves of the short vegetal fiber-filled filaments are presented in Figure 3b. The residues at the end of the heating process could be used to prove the presence of the reinforcements. The tomato, pruned orange, hemp, and weed vegetal fiber contents in filaments were 2.93 wt%, 6.94 wt%, 3.75 wt%, and 7.09 wt%, respectively.

3.2. Anisotropic Mechanical Behaviors

The tensile behaviors of the WVFFPBs with different print orientations are shown in Figure 4. The performance difference of the 3D-printed samples in both directions 0° and 90° was significant [28]; therefore, the anisotropic mechanical properties of printed PLA and WVFFPBs in these two directions were compared. As shown in Table 2, the anisotropic mechanical properties of WVFFPBs in the 0° and 90° directions were significantly higher than those of pristine PLA samples. The PLA samples printed in the 0° and 90° directions showed similar elongation at break (0%), with a 45.2% difference in peak load. Comparatively, the WVFFPB samples printed in the 0° and 90° directions showed significant differences in elongation at break and peak load. Taking weed vegetal fiber-filled composites as an example, the elongation at break and peak load of the printed samples in both directions differed by 45.8% and 69.4%, respectively, as shown in Table 2. Compared to pristine PLA samples, the WVFFPBs exhibited better anisotropic mechanical behaviors, but the peak load was smaller than PLA samples due to the large number of pores caused by the addition of short vegetal fibers.
In order to further investigate the anisotropic mechanical behavior of 3D-printed WVFFPBs at different print orientations, the short pruned and weed vegetal fiber-filled composites printed at 0°–90° were selected as representatives for the study. As shown in Figure 5, the print orientation had a significant influence on the mechanical behavior of WVFFPBs, with samples printed in the 0° direction exhibiting the highest values of load and elongation at break. The short pruned vegetal fiber-filled composites exhibited the worst elongation at break and load values when printed at a 75° orientation, as shown in Figure 5a. Comparatively, the short weed vegetal fiber-filled composites showed the worst elongation at break and load values when printed at 90° and 75° orientations, respectively, as shown in Figure 5b. In addition, the load–displacement curves of short pruned vegetal fiber-filled composites with various print orientations showed significant differences compared to weed vegetal fiber-filled composites, resulting in a better anisotropic mechanical property.
A summary of pristine PLA and pruned fiber-filled composite tensile test results appears in Figure 6. The tensile strength and elongation at break of the PLA samples in different print orientations were higher than those of the short pruned fiber-filled composites. Note that the addition of pruned fibers brought a large number of pores, resulting in a decrease in the mechanical properties of the pruned fiber-filled composites. As the print orientation changed, the pruned fiber-filled composites exhibited significant anisotropic mechanical properties compared to the PLA samples. For instance, the tensile strength of pruned fiber-filled composites printed at 45° and 30° orientations were 8.77 MPa and 14.09 MPa, respectively, a difference of 37.8%. Furthermore, the fracture displacement difference between the two was 45.9%, although the printing angle only differed by 15°, as shown in Figure 6.
A summary of pristine PLA and short weed fiber-filled composite tensile test results appears in Figure 7. As the printing angle increased, the tensile mechanical properties of the samples showed a decreasing trend [29,30]. Similarly, the tensile strength and elongation at break of the PLA samples in different print orientations were higher than those of the short weed fiber-filled composites. However, the short weed fiber-filled composites showed better anisotropic mechanical properties when the print orientation of the sample changed. Taking 30° and 45° orientations for the printed samples as an example, the differences in tensile strength and elongation at break of the pristine PLA samples were 3.5% and 22.8%, respectively. Comparatively, the differences in tensile strength and elongation at break of the weed fiber-filled composites printed in these two orientations were 17.3% and 26.5%, respectively, as shown in Figure 7.

3.3. Damage Behaviors

The optical microscope images for the damage characteristics of the 0°, 30°, 60°, and 90° printed pruned fiber-filled composites are presented in Figure 8. As shown in Figure 8, as the printing angle increased, more cracks appeared between the deposition lines of the sample, resulting in a large number of cracks appearing on the surface of the 90° print orientation sample. The fracture damage of the sample was controlled by the print orientation, and samples with different printing angles exhibited different fracture morphologies. The sample printed in the 0° direction fractured perpendicular to the printing direction, with a serrated fracture shape [31,32,33]. Observing the fracture surface, it was found that there were obvious pores between the deposition lines. The sample printed in the 30° direction fractured along the printing direction, and the matrix on the fractured surface experienced severe shear failure. Comparatively, the samples printed at 60° and 90° also fractured along the printing direction, but the matrix on the fracture surface did not show significant shear failure, which was attributed to the obvious cracks generated between the deposition lines.
The optical microscope images for the damage characteristics of the weed fiber-filled composites printed at different angles are presented in Figure 9. Similar to the pruned fiber-filled composites, the fracture damage of the sample was affected by the print orientation, and samples with different printing angles exhibited different fracture modes. However, the weed fiber-filled composite sample printed in the 30° direction fractured along the printing direction with a serrated fracture surface, indicating that the bonding performance between deposition lines of the weed fiber-filled composite was better than that of the pruned fiber-filled composite sample. In addition, the deposition line cracks of samples printed at 60° and 90° were also decreased, and the fracture surface of samples printed at 60° also experienced matrix shear failure. Therefore, the forming quality of weed fiber-filled composites was significantly better than that of pruned fiber-filled composites, thus exhibiting better mechanical properties (Figure 5).
As shown in Figure 10, the short weed fiber-filled composites printed with different printing angles were selected to further study the microscopic failure mode of the samples after tension. Compared with the 3D printing filament, the porosity of the printed sample was significantly reduced (Figure 2 and Figure 10). However, a large number of prismatic holes between deposited lines appeared in the printed samples. Under the tensile load, samples with different printing angles exhibited different forms of fracture damage. The fracture surface of the sample printed with 0° showed serious matrix deformation and presented fewer pores (Figure 10e,i). The fracture mode of samples with printing angles of 30°, 60°, and 90° was a mixed mode of interlayer delamination and deposited line fracture (Figure 10b–d,f–h). As shown in Figure 10j–l, there were numerous pores on the fracture surfaces of deposited lines. This could be attributed to the fact that the position with more pores in the sample had the worst mechanical properties and was more prone to fracture.

4. Conclusions

In this work, waste tomato, pruned orange, hemp, and weed vegetal fiber-filled PLA-based biocomposites with different print orientations were successfully developed through the 3D printing method. The anisotropic mechanical behaviors of waste vegetal fiber-filled polymer biocomposites (WVFFPBs) and pristine PLA matrix samples under tensile load were compared. Based on the obtained results, the following conclusions were drawn.
The anisotropic mechanical properties of WVFFPBs in the 0° and 90° directions were significantly higher than those of the pristine PLA samples. The PLA samples printed in the 0° and 90° directions showed similar elongation at break (0%), with a 45.2% difference in peak load. Comparatively, taking weed vegetal fiber-filled composites as an example, the elongation at break and peak load of the printed samples in both directions differed by 45.8% and 69.4%, respectively. The WVFFPBs exhibited better anisotropic mechanical behaviors, but the peak load was smaller than that of the PLA samples due to the large number of pores caused by the addition of short vegetal fibers.
As the printing angle increased (0°–90°, increased by 15° each time), the tensile mechanical properties of the WVFFPBs showed a decreasing trend. The biocomposites showed significant anisotropic mechanical properties compared to the PLA samples when the print orientation increased. For instance, the tensile strength of pruned fiber-filled composites printed at 45° and 30° orientations were 8.77 MPa and 14.09 MPa, respectively, a difference of 37.8%. In addition, the fracture damage of the WVFFPBs was controlled by the print orientation, and samples with different printing angles exhibited different fracture morphologies.
In addition, the study of 3D printing parameters and the environment on the natural degradation performance of 3D-printed WVFFPBs was very meaningful. In future work, the natural degradation performance of 3D-printed short vegetal fiber-filled biocomposites will be investigated.

Author Contributions

Conceptualization, H.W. and P.C.; methodology, H.W., P.C., Y.L. and Z.F.; validation. Y.L., P.C. and K.W.; investigation, K.W. and Y.P.; data curation, Y.L. and Z.F.; writing—original draft preparation, P.C.; writing—review and editing, P.C.; funding acquisition, K.W. and Y.P. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Hunan Science Foundation for Distinguished Young Scholars of China, grant number 2021JJ10059, and the First Batch of 2021 MOE of PRC Industry–University Collaborative Education Program, grant number 202107ZCJG05. The author Ping Cheng gratefully acknowledges financial support from the China Scholarship Council, grant number 202206370135.

Data Availability Statement

The data presented in this study are available on request from the corresponding author.

Acknowledgments

The authors would like to show sincere thanks to the technicians who contributed to this research.

Conflicts of Interest

Authors Honggang Wang, Zhi Fu and Yu Liu was employed by the company China Automotive Engineering Research Institute Co., Ltd. The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

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Figure 1. Schematic representations of the (a) 3D printer and (b) print orientation of the sample.
Figure 1. Schematic representations of the (a) 3D printer and (b) print orientation of the sample.
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Figure 2. Microscopic images of short (a–d) tomato and (e–h) hemp vegetal fiber-filled filaments.
Figure 2. Microscopic images of short (a–d) tomato and (e–h) hemp vegetal fiber-filled filaments.
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Figure 3. (a) Tensile strength and (b) thermogravimetric curves of different short vegetal fiber-filled filaments.
Figure 3. (a) Tensile strength and (b) thermogravimetric curves of different short vegetal fiber-filled filaments.
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Figure 4. Load–displacement curves with 0° and 90° orientations of short (a) tomato, (b) pruned, (c) hemp, and (d) weed vegetal fiber-filled composites.
Figure 4. Load–displacement curves with 0° and 90° orientations of short (a) tomato, (b) pruned, (c) hemp, and (d) weed vegetal fiber-filled composites.
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Figure 5. Load–displacement curves with different orientations of short (a) pruned and (b) weed vegetal fiber-filled composites.
Figure 5. Load–displacement curves with different orientations of short (a) pruned and (b) weed vegetal fiber-filled composites.
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Figure 6. (a) Tensile strength and (b) elongation at break of pristine PLA and short pruned fiber-filled composites.
Figure 6. (a) Tensile strength and (b) elongation at break of pristine PLA and short pruned fiber-filled composites.
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Figure 7. (a) Tensile strength and (b) elongation at break of pristine PLA and short weed fiber-filled composites.
Figure 7. (a) Tensile strength and (b) elongation at break of pristine PLA and short weed fiber-filled composites.
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Figure 8. Macro images for fracture surfaces of short pruned fiber-filled composites with different printing angles.
Figure 8. Macro images for fracture surfaces of short pruned fiber-filled composites with different printing angles.
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Figure 9. Macro images for fracture surfaces of short weed fiber-filled composites with different printing angles.
Figure 9. Macro images for fracture surfaces of short weed fiber-filled composites with different printing angles.
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Figure 10. SEM images of fracture surfaces of short weed fiber-filled composites with (a,e,i) 0°, (b,f,j) 30°, (c,g,k) 60° and (d,h,l) 90° printing angles.
Figure 10. SEM images of fracture surfaces of short weed fiber-filled composites with (a,e,i) 0°, (b,f,j) 30°, (c,g,k) 60° and (d,h,l) 90° printing angles.
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Table 1. Material parameters of short vegetal fiber-filled PLA filaments.
Table 1. Material parameters of short vegetal fiber-filled PLA filaments.
Fiber TypeManufacturerFiber
Dimensions		Printing
Temperature		Layer
Thickness
TomatoKanèsis300 μm185 °C0.2 mm
Pruned Orange
Hemp
Weed
Table 2. Summaries of anisotropic mechanical properties for 0° and 90° print orientations.
Table 2. Summaries of anisotropic mechanical properties for 0° and 90° print orientations.
PropertyOrientationPLATomato PrunedHempWeed
EB 1
(%)		0°0.88 ± 0.080.70 ± 0.030.98 ± 0.060.70 ± 0.090.83 ± 0.09
90°0.88 ± 0.020.51 ± 0.070.61 ± 0.020.44 ± 0.030.45 ± 0.10
D 2 0%27.1%37.8%37.13%45.8%
PL 3
(kN)		0°0.73 ± 0.060.44 ± 0.050.41 ± 0.060.47 ± 0.010.62 ± 0.02
90°0.40 ± 0.020.12 ± 0.090.13 ± 0.040.16 ± 0.050.19 ± 0.03
D 45.2%72.7%65.1%66.0%69.4%
1 Elongation at break, 2 difference, 3 peak load.
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Wang, H.; Fu, Z.; Liu, Y.; Cheng, P.; Wang, K.; Peng, Y. Exploring Anisotropic Mechanical Characteristics in 3D-Printed Polymer Biocomposites Filled with Waste Vegetal Fibers. Symmetry 2024, 16, 70. https://doi.org/10.3390/sym16010070

AMA Style

Wang H, Fu Z, Liu Y, Cheng P, Wang K, Peng Y. Exploring Anisotropic Mechanical Characteristics in 3D-Printed Polymer Biocomposites Filled with Waste Vegetal Fibers. Symmetry. 2024; 16(1):70. https://doi.org/10.3390/sym16010070

Chicago/Turabian Style

Wang, Honggang, Zhi Fu, Yu Liu, Ping Cheng, Kui Wang, and Yong Peng. 2024. "Exploring Anisotropic Mechanical Characteristics in 3D-Printed Polymer Biocomposites Filled with Waste Vegetal Fibers" Symmetry 16, no. 1: 70. https://doi.org/10.3390/sym16010070

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