J. Mater. Sci. Technol. ›› 2022, Vol. 121: 52-66.DOI: 10.1016/j.jmst.2021.11.064
• Research Article • Previous Articles Next Articles
Sithiprumnea Dula,*(
), Brenda J. Alonso Gutierrezb,c, Alessandro Pegorettia, Jaime Alvarez-Quintanab, Luca Fambria,*()
Received:2021-07-31
Revised:2021-11-04
Accepted:2021-11-06
Published:2022-09-10
Online:2022-03-08
Contact:
Sithiprumnea Dul,Luca Fambri
About author:*E-mail addresses: sithiprumnea.dul@unitn.it (S. Dul),Sithiprumnea Dul, Brenda J. Alonso Gutierrez, Alessandro Pegoretti, Jaime Alvarez-Quintana, Luca Fambri. 3D printing of ABS Nanocomposites. Comparison of processing and effects of multi-wall and single-wall carbon nanotubes on thermal, mechanical and electrical properties[J]. J. Mater. Sci. Technol., 2022, 121: 52-66.
Fig. 1. Number of publications in the field of additive manufacturing and its integration with composites and nanocomposites from Web of ScienceTM in the last decade (up to October 30th, 2021).
| Nanoparticle | Manufacturer | Density (g/cm3) | Length (μm) | Diameter (nm) | Aspect ratio | Surface area (m2/g) | Carbon purity (%) |
|---|---|---|---|---|---|---|---|
| MWCNT-NC7000 | Nanocyl, Belgium | 2.15 ± 0.03* | 1.5 | 9.5 | 158 | 250-300 | >90 |
| SWCNT-TUBALL | TUBALL, USA | 1.877** | 5 | 1.6 ± 0.4 | 3125 | >300 | >80 |
Table 1. Properties of commercial single-walled and multi-walled carbon nanotubes according to the manufacturer.
| Nanoparticle | Manufacturer | Density (g/cm3) | Length (μm) | Diameter (nm) | Aspect ratio | Surface area (m2/g) | Carbon purity (%) |
|---|---|---|---|---|---|---|---|
| MWCNT-NC7000 | Nanocyl, Belgium | 2.15 ± 0.03* | 1.5 | 9.5 | 158 | 250-300 | >90 |
| SWCNT-TUBALL | TUBALL, USA | 1.877** | 5 | 1.6 ± 0.4 | 3125 | >300 | >80 |
Fig. 2. SEM micrographs of MWCNT (a) and SWCNT (b).
Fig. 3. Comparative Raman spectra of MWCNT and SWCNT.
Fig. 4. ABS/MWCNT (M) and ABS/SWCNT (S) fibers at different wt.% CNT content, freely extruded from the nozzle of a 3D printer.
Fig. 5. (a) 3D model of 1BA dumbbells (thickness of 2 mm and 0.6 mm) and plate (30 × 5 × 2 mm3), (b) the arrangement of dumbbells, (c) the detail of infill pattern [+45°/-45°] and (d) 3D-printed samples.
| Samples | X (mm) | Y (mm) | Z (mm) | Deposition time of a single layer (s) | Number of layers | Total time (min) | Analysis |
|---|---|---|---|---|---|---|---|
| Dumbbell 1 | 75 | 5-10a | 2 | 145 | 10 | 24.2 | Tensile |
| Dumbbell 2 | 75 | 5-10a | 0.6 | 145 | 3 | 7.3 | Creep |
| Dumbbell 3 | 75 | 5-10a | 0.6 | 145 | 1 | 2.4 | Resistivity |
| Parallelepiped | 30 | 5 | 2 | 55 | 10 | 9.2 | Density, VST and resistivity |
Table 2. Dimensions, geometrical parameters in production, and analysis of FFF specimens.
| Samples | X (mm) | Y (mm) | Z (mm) | Deposition time of a single layer (s) | Number of layers | Total time (min) | Analysis |
|---|---|---|---|---|---|---|---|
| Dumbbell 1 | 75 | 5-10a | 2 | 145 | 10 | 24.2 | Tensile |
| Dumbbell 2 | 75 | 5-10a | 0.6 | 145 | 3 | 7.3 | Creep |
| Dumbbell 3 | 75 | 5-10a | 0.6 | 145 | 1 | 2.4 | Resistivity |
| Parallelepiped | 30 | 5 | 2 | 55 | 10 | 9.2 | Density, VST and resistivity |
| Parameter | Value |
|---|---|
| Nozzle diameter | 0.4 mm |
| Nozzle temperature | 280 °C |
| Bed temperature | 110 °C |
| Nozzle speed | 40 mm/s |
| Layer height | 0.2 mm |
| Raster angle | +45°/-45° |
| Infill density | 100% |
| Number of contours | 2 |
Table 3. 3D printing parameters by fused filament fabrication technique for specimen's production.
| Parameter | Value |
|---|---|
| Nozzle diameter | 0.4 mm |
| Nozzle temperature | 280 °C |
| Bed temperature | 110 °C |
| Nozzle speed | 40 mm/s |
| Layer height | 0.2 mm |
| Raster angle | +45°/-45° |
| Infill density | 100% |
| Number of contours | 2 |
Fig. 6. Schematic illustration of resistivity measurement: (a) four-probes method and (b) two-probes method.
| Samples | Filament diameter (mm) | Fibers diameter (μm) | Skirt**diameter (μm) | Filament linear density (tex) | Fiber linear density (tex) | Skirt linear density (tex) | Feeding OFFeed | Spinning OFSpin | Swelling SWSpin | Total OFTot | DRSpin |
|---|---|---|---|---|---|---|---|---|---|---|---|
| ABS* | 1725 ± 14 | 648 ± 21 | // | 2433 | 343 | // | 18.6 | 0.38 | 2.6 | 7.1 | // |
| M5 | 1772 ± 13 | 450 ± 1 | 275 | 2637 | 170 | 63 | 19.6 | 0.79 | 1.3 | 15.5 | 2.7 |
| M7.5 | 1783 ± 7 | 448 ± 2 | 274 | 2704 | 171 | 64 | 19.9 | 0.80 | 1.3 | 15.9 | 2.7 |
| M10 | 1782 ± 31 | 424 ± 3 | 281 | 2739 | 155 | 68 | 19.9 | 0.89 | 1.1 | 17.6 | 2.3 |
| S5 | 1744 ± 16 | 419 ± 3 | 282 | 2543 | 147 | 66 | 19.0 | 0.91 | 1.1 | 17.3 | 2.2 |
| S7.5 | 1795 ± 1 | 410 ± 2 | 271 | 2725 | 142 | 62 | 20.1 | 0.95 | 1.1 | 19.2 | 2.3 |
| S10 | 1779 ± 10 | 396 ± 5 | 277 | 2710 | 134 | 66 | 19.8 | 1.02 | 1.0 | 20.2 | 2.0 |
Table 4. Dimension and linear density of various extrudates produced from ABS and its nanocomposites, i.e. filaments (from single screw extruder), fibers and skirt (from 3D printing). Orientation factors OF and draw ratio DR during 3D extrusion calculated according to Equations 1 - 5.
| Samples | Filament diameter (mm) | Fibers diameter (μm) | Skirt**diameter (μm) | Filament linear density (tex) | Fiber linear density (tex) | Skirt linear density (tex) | Feeding OFFeed | Spinning OFSpin | Swelling SWSpin | Total OFTot | DRSpin |
|---|---|---|---|---|---|---|---|---|---|---|---|
| ABS* | 1725 ± 14 | 648 ± 21 | // | 2433 | 343 | // | 18.6 | 0.38 | 2.6 | 7.1 | // |
| M5 | 1772 ± 13 | 450 ± 1 | 275 | 2637 | 170 | 63 | 19.6 | 0.79 | 1.3 | 15.5 | 2.7 |
| M7.5 | 1783 ± 7 | 448 ± 2 | 274 | 2704 | 171 | 64 | 19.9 | 0.80 | 1.3 | 15.9 | 2.7 |
| M10 | 1782 ± 31 | 424 ± 3 | 281 | 2739 | 155 | 68 | 19.9 | 0.89 | 1.1 | 17.6 | 2.3 |
| S5 | 1744 ± 16 | 419 ± 3 | 282 | 2543 | 147 | 66 | 19.0 | 0.91 | 1.1 | 17.3 | 2.2 |
| S7.5 | 1795 ± 1 | 410 ± 2 | 271 | 2725 | 142 | 62 | 20.1 | 0.95 | 1.1 | 19.2 | 2.3 |
| S10 | 1779 ± 10 | 396 ± 5 | 277 | 2710 | 134 | 66 | 19.8 | 1.02 | 1.0 | 20.2 | 2.0 |
Fig. 7. FESEM micrographs of ABS/MWCNT composites: M7-3D (a, b) and M10-3D samples (c, d).
Fig. 8. FESEM micrographs of ABS/SWCNT composites: S7 - 3D (a, b) and S10-3D (c, d).
| Samples | CNT vol. (%) | Apparent density (g/cm3) | Theoreticaldensity (g/cm3) | VV (%) |
|---|---|---|---|---|
| ABS-3D | 0.00 | 0.98 ± 0.01 | 1.041 | 6.2 ± 0.9 |
| M5-3D | 2.48 | 1.00 ± 0.01 | 1.069 | 6.3 ± 0.9 |
| M7.5-3D | 3.78 | 0.99 ± 0.01 | 1.083 | 8.8 ± 1.0 |
| M10-3D | 5.10 | 1.01 ± 0.01 | 1.098 | 8.3 ± 1.0 |
| S5-3D | 2.84 | 0.98 ± 0.01 | 1.065 | 8.4 ± 1.0 |
| S7.5-3D | 4.30 | 0.99 ± 0.01 | 1.077 | 7.7 ± 1.0 |
| S10-3D | 5.80 | 0.99 ± 0.01 | 1.090 | 8.8 ± 0.6 |
Table 5. Composition of 3D printed ABS and its nanocomposites (in percentage by wt. %). Density and a void fraction (Vv) as a function of CNT content.
| Samples | CNT vol. (%) | Apparent density (g/cm3) | Theoreticaldensity (g/cm3) | VV (%) |
|---|---|---|---|---|
| ABS-3D | 0.00 | 0.98 ± 0.01 | 1.041 | 6.2 ± 0.9 |
| M5-3D | 2.48 | 1.00 ± 0.01 | 1.069 | 6.3 ± 0.9 |
| M7.5-3D | 3.78 | 0.99 ± 0.01 | 1.083 | 8.8 ± 1.0 |
| M10-3D | 5.10 | 1.01 ± 0.01 | 1.098 | 8.3 ± 1.0 |
| S5-3D | 2.84 | 0.98 ± 0.01 | 1.065 | 8.4 ± 1.0 |
| S7.5-3D | 4.30 | 0.99 ± 0.01 | 1.077 | 7.7 ± 1.0 |
| S10-3D | 5.80 | 0.99 ± 0.01 | 1.090 | 8.8 ± 0.6 |
| Samples | CNT vol. (%) | VSTTop (°C) | VSTBottom (°C) | Tg* (°C) | VST -Tg** (°C) |
|---|---|---|---|---|---|
| ABS-3D | 0.00 | 111.9 ± 0.7 | 110.9 ± 0.7 | 107.1 | 4.4 |
| M5-3D | 2.48 | 114.4 ± 0.7 | 114.2 ± 1.0 | 109.1 | 5.3 |
| M7.5-3D | 3.78 | 114.4 ± 1.0 | 113.8 ± 1.0 | 109.1 | 5.1 |
| M10-3D | 5.10 | 118.6 ± 1.1 | 117.4 ± 0.3 | 109.7 | 8.3 |
| S5-3D | 2.84 | 123.2 ± 0.8 | 121.7 ± 1.4 | 109.5 | 13.0 |
| S7.5-3D | 4.30 | 126.7 ± 0.3 | 125.5 ± 1.4 | 109.5 | 16.7 |
| S10-3D | 5.80 | 129.4 ± 1.4 | 129.0 ± 1.3 | 108.8 | 20.4 |
Table 6. Vicat Softening Temperature (VST) of ABS and its nanocomposites as a function of wt. % composition.
| Samples | CNT vol. (%) | VSTTop (°C) | VSTBottom (°C) | Tg* (°C) | VST -Tg** (°C) |
|---|---|---|---|---|---|
| ABS-3D | 0.00 | 111.9 ± 0.7 | 110.9 ± 0.7 | 107.1 | 4.4 |
| M5-3D | 2.48 | 114.4 ± 0.7 | 114.2 ± 1.0 | 109.1 | 5.3 |
| M7.5-3D | 3.78 | 114.4 ± 1.0 | 113.8 ± 1.0 | 109.1 | 5.1 |
| M10-3D | 5.10 | 118.6 ± 1.1 | 117.4 ± 0.3 | 109.7 | 8.3 |
| S5-3D | 2.84 | 123.2 ± 0.8 | 121.7 ± 1.4 | 109.5 | 13.0 |
| S7.5-3D | 4.30 | 126.7 ± 0.3 | 125.5 ± 1.4 | 109.5 | 16.7 |
| S10-3D | 5.80 | 129.4 ± 1.4 | 129.0 ± 1.3 | 108.8 | 20.4 |
Fig. 9. Vicat thermograms of tip penetration in 3D printed ABS/CNT nanocomposites - upper surface. (load 10 N; heating rate 2 °C/min).
Fig. 10. TGA and DTGA curves of nanofilled ABS/MWCNT (a, b) and ABS/SWCNT (c, d) filaments under nitrogen atmosphere.
| Samples | Mass Loss (%) at 280 °C | Tonset (°C) | Td,max (°C) | MMLR (%/°C) | Residue(%) | ||
|---|---|---|---|---|---|---|---|
| Empty Cell | Empty Cell | Empty Cell | Empty Cell | Empty Cell | at 475 °C | at 575 °C | at 700 °C |
| ABS-3D | 0.52 | 414.6 | 433.3 | 2.15 | 2.8 | 0.6 | 0.0 |
| M5-3D | 0.55 | 412.7 | 435.2 | 1.77 | 10.7 | 6.5 | 6.0 |
| M7.5-3D | 0.27 | 412.3 | 433.3 | 1.73 | 13.4 | 9.3 | 9.0 |
| M10-3D | 0.48 | 409.2 | 430.2 | 1.64 | 15.2 | 11.7 | 11.4 |
| S5-3D | 0.35 | 412.7 | 436.0 | 1.77 | 11.5 | 7.5 | 7.1 |
| S7.5-3D | 0.62 | 415.7 | 435.8 | 1.78 | 13.5 | 9.6 | 9.3 |
| S10-3D | 0.37 | 407.5 | 432.5 | 1.70 | 16.0 | 12.5 | 12.2 |
| MWCNT | - | - | - | - | 96.4 | 95.6 | 94.1 |
| SWCNT | - | - | - | - | 96.2 | 95.5 | 94.5 |
Table 7. TGA data of pure 3D-printed nanocomposite in a nitrogen atmosphere.
| Samples | Mass Loss (%) at 280 °C | Tonset (°C) | Td,max (°C) | MMLR (%/°C) | Residue(%) | ||
|---|---|---|---|---|---|---|---|
| Empty Cell | Empty Cell | Empty Cell | Empty Cell | Empty Cell | at 475 °C | at 575 °C | at 700 °C |
| ABS-3D | 0.52 | 414.6 | 433.3 | 2.15 | 2.8 | 0.6 | 0.0 |
| M5-3D | 0.55 | 412.7 | 435.2 | 1.77 | 10.7 | 6.5 | 6.0 |
| M7.5-3D | 0.27 | 412.3 | 433.3 | 1.73 | 13.4 | 9.3 | 9.0 |
| M10-3D | 0.48 | 409.2 | 430.2 | 1.64 | 15.2 | 11.7 | 11.4 |
| S5-3D | 0.35 | 412.7 | 436.0 | 1.77 | 11.5 | 7.5 | 7.1 |
| S7.5-3D | 0.62 | 415.7 | 435.8 | 1.78 | 13.5 | 9.6 | 9.3 |
| S10-3D | 0.37 | 407.5 | 432.5 | 1.70 | 16.0 | 12.5 | 12.2 |
| MWCNT | - | - | - | - | 96.4 | 95.6 | 94.1 |
| SWCNT | - | - | - | - | 96.2 | 95.5 | 94.5 |
Fig. 11. Representative stress-strain curves of ABS nanocomposites 3D-printed samples containing MWCNT (full symbol) and SWCNT (open symbol).
| Samples | Tensile modulus E (MPa) | Yield stress σy (MPa) | Yield strain εy (%) | Stress at break σb (MPa) | Elongation at break εb (%) | Tensile Energy to break TEB (MJ/m3) | Normalized Modulus* (--) |
|---|---|---|---|---|---|---|---|
| ABS-3D | 2278 ± 118 | 38.0 ± 1.3 | 5.2 ± 0.4 | 31.2 ± 0.8 | 13.9 ± 3.1 | 4.09 ± 1.13 | n.d. |
| M5-3D | 2429 ± 194 | 42.5 ± 1.4 | 4.3 ± 0.2 | 38.4 ± 1.3 | 5.6 ± 0.4 | 1.60 ± 0.19 | 1.3 |
| M7.5-3D | 3119 ± 110 | - | - | 46.6 ± 2.6 | 4.2 ± 0.6 | 1.16 ± 0.28 | 4.9 |
| M10-3D | 3213 ± 13 | - | - | 45.0 ± 4.6 | 3.6 ± 0.5 | 0.95 ± 0.25 | 4.1 |
| S5-3D | 3507 ± 183 | - | - | 38.7 ± 3.0 | 2.9 ± 0.4 | 0.59 ± 0.11 | 10.8 |
| S7.5-3D | 6434 ± 254 | - | - | 40.5 ± 2.5 | 2.6 ± 0.2 | 0.59 ± 0.09 | 24.3 |
| S10-3D | 7045 ± 261 | - | - | 40.3 ± 2.2 | 1.8 ± 0.1 | 0.40 ± 0.03 | 20.9 |
Table 8. Comparison of the tensile properties of ABS/SWCNT and ABS/MWCNT nanocomposites of 3D-printed samples.
| Samples | Tensile modulus E (MPa) | Yield stress σy (MPa) | Yield strain εy (%) | Stress at break σb (MPa) | Elongation at break εb (%) | Tensile Energy to break TEB (MJ/m3) | Normalized Modulus* (--) |
|---|---|---|---|---|---|---|---|
| ABS-3D | 2278 ± 118 | 38.0 ± 1.3 | 5.2 ± 0.4 | 31.2 ± 0.8 | 13.9 ± 3.1 | 4.09 ± 1.13 | n.d. |
| M5-3D | 2429 ± 194 | 42.5 ± 1.4 | 4.3 ± 0.2 | 38.4 ± 1.3 | 5.6 ± 0.4 | 1.60 ± 0.19 | 1.3 |
| M7.5-3D | 3119 ± 110 | - | - | 46.6 ± 2.6 | 4.2 ± 0.6 | 1.16 ± 0.28 | 4.9 |
| M10-3D | 3213 ± 13 | - | - | 45.0 ± 4.6 | 3.6 ± 0.5 | 0.95 ± 0.25 | 4.1 |
| S5-3D | 3507 ± 183 | - | - | 38.7 ± 3.0 | 2.9 ± 0.4 | 0.59 ± 0.11 | 10.8 |
| S7.5-3D | 6434 ± 254 | - | - | 40.5 ± 2.5 | 2.6 ± 0.2 | 0.59 ± 0.09 | 24.3 |
| S10-3D | 7045 ± 261 | - | - | 40.3 ± 2.2 | 1.8 ± 0.1 | 0.40 ± 0.03 | 20.9 |
Fig. 12. Elastic modulus of nanocomposites ABS/MWCNT (a) and ABS/SWCNT (b). Continuous (___) and dash lines (_ _ _) and dot lines (…) represent prediction according to the Halpin‐Tsai models with parallel, 2D random and 3D random orientation, respectively.
Fig. 13. Normalized modulus of 3D-printed nanocomposites, as a function of different carbonaceous wt.% content. ABS/MWCNT and ABS/SWCNT of the present study compared to literature data, such as CF in ABS [44,45] and in PA [46]; r-GO in PLA[7]; CNT in PEEK[18], PLA [47] and in ABS [25,48].
Fig. 14. Creep compliance, D(t) of 3D-printed neat ABS, ABS/MWCNT and ABS/SWCNT samples at 3.0 MPa at a temperature of 30 °C.
| Samples | Del (GPa-1) | Dve, 3600s (GPa-1) | Dtot, 3600s (GPa-1) | De (GPa-1) | k (GPa-1s-n) | n | R |
|---|---|---|---|---|---|---|---|
| ABS-3D | 0.728 | 0.262 | 0.989 | 0.786 | 0.035 | 0.214 | 0.994 |
| M5-3D | 0.696 | 0.235 | 0.931 | 0.759 | 0.018 | 0.279 | 0.995 |
| M7.5-3D | 0.658 | 0.203 | 0.861 | 0.726 | 0.009 | 0.328 | 0.989 |
| M10-3D | 0.621 | 0.209 | 0.830 | 0.681 | 0.011 | 0.319 | 0.995 |
| S5-3D | 0.523 | 0.210 | 0.733 | 0.540 | 0.054 | 0.152 | 0.988 |
| S7.5-3D | 0.407 | 0.148 | 0.555 | 0.424 | 0.007 | 0.366 | 0.994 |
| S10-3D | 0.259 | 0.011 | 0.372 | 0.298 | 0.008 | 0.265 | 0.928 |
Table 9. Creep test of neat ABS and its nanocomposites as measured on 3D-printed samples and fitting parameters (Equation (18)).
| Samples | Del (GPa-1) | Dve, 3600s (GPa-1) | Dtot, 3600s (GPa-1) | De (GPa-1) | k (GPa-1s-n) | n | R |
|---|---|---|---|---|---|---|---|
| ABS-3D | 0.728 | 0.262 | 0.989 | 0.786 | 0.035 | 0.214 | 0.994 |
| M5-3D | 0.696 | 0.235 | 0.931 | 0.759 | 0.018 | 0.279 | 0.995 |
| M7.5-3D | 0.658 | 0.203 | 0.861 | 0.726 | 0.009 | 0.328 | 0.989 |
| M10-3D | 0.621 | 0.209 | 0.830 | 0.681 | 0.011 | 0.319 | 0.995 |
| S5-3D | 0.523 | 0.210 | 0.733 | 0.540 | 0.054 | 0.152 | 0.988 |
| S7.5-3D | 0.407 | 0.148 | 0.555 | 0.424 | 0.007 | 0.366 | 0.994 |
| S10-3D | 0.259 | 0.011 | 0.372 | 0.298 | 0.008 | 0.265 | 0.928 |
Fig. 15. Volume electrical resistivity in (Ω cm) of ABS nanocomposite of filaments, 3D-printed samples infill [± 45°] (1 layer and 10 layers) and Skirt [0°] by four-probe method (a) and 3D-printed samples infill [± 45°] 10 layers in XY-direction and Z-direction by two probe method (b).
| Samples | Tensile modulus (%) | Stress at Break (%) | Elongation at Break (%) | VST (%) | Conductivity (%) |
|---|---|---|---|---|---|
| ABS | 103 | 89 | 54 | 100 | // |
| M5 | 100 | 97 | 160 | 101 | 0.4 |
| M7.5 | 120 | 99 | 127 | 99 | 4.9 |
| M10 | 116 | 95 | 138 | 102 | 20.9 |
| S5 | 67 | 74 | 207 | 102 | 0.4 |
| S7.5 | 95 | 75 | 236 | 102 | 0.3 |
| S10 | 114 | 74 | 150 | 98 | 0.6 |
Table 10. Comparison of relative properties of 3D-printed samples versus extruded filaments or plates (VST), as a function of MWCNT and SWCNT in ABS nanocomposites, according to Eq.19.
| Samples | Tensile modulus (%) | Stress at Break (%) | Elongation at Break (%) | VST (%) | Conductivity (%) |
|---|---|---|---|---|---|
| ABS | 103 | 89 | 54 | 100 | // |
| M5 | 100 | 97 | 160 | 101 | 0.4 |
| M7.5 | 120 | 99 | 127 | 99 | 4.9 |
| M10 | 116 | 95 | 138 | 102 | 20.9 |
| S5 | 67 | 74 | 207 | 102 | 0.4 |
| S7.5 | 95 | 75 | 236 | 102 | 0.3 |
| S10 | 114 | 74 | 150 | 98 | 0.6 |
Fig. 16. Comparison of selected properties of ABS/MWCNT and ABS/SWCNT 3D-printed nanocomposites as a function of nanofiller content (5-10 wt. %).
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