Analyzing Parameters of Pure and Reinforced 3D Printed PLA and ABS Samples

If you want high-quality 3D printed parts, then you need to choose the right print parameters. Research on this topic is ongoing, and the latest comes from the University of Manchester. Chamil Abeykoon, Pimpisut Sri-Amphorn, and Anura Fernando, with the Northwest Composite Centre in the Aerospace Research Institute, published “Optimization of fused deposition modeling parameters for improved PLA and ABS 3D printed structures,” about their work studying various properties and processing conditions of 3D printed specimens made with different materials.

There are multiple variables involved in 3D printing, and changing just one parameter could cause “consequential changes in several other parameters” at the same time. Additionally, the most commonly used FDM printing materials are thermoplastic polymers with low melting points – not ideal for “some high performance applications.”

“Therefore, attempts have been made to improve the properties of printing filaments by adding particles such as short-fibres, nanoparticles and other suitable additives [18]. Thanks to these extensive researches and developments in the area of FDM, fibre-reinforced filaments are becoming popular and are currently available for practical applications,” they explained.

In order to optimize parameters and settings for these new reinforced materials, the team says we need more 3D printing research and development. In their study, they investigated the process using seven infill patterns, five print speeds, and four set nozzle temperatures, and observed and analyzed the mechanical, thermal, and morphological properties.

They used five commercially available materials, with 1.75 mm diameters:

  • Polylactic acid (PLA)
  • Acrylonitrile butadiene styrene (ABS)
  • Carbon fiber-reinforced PLA (CFR-PLA)
  • Carbon fiber-reinforced ABS (CFR-ABS)
  • Carbon nanotube-reinforced ABS (CNT-ABS)

The samples were designed with SOLIDWORKS and printed on a MakerBot Replicator 2, MakerBot Replicator 2X, and MakerBot Replicator Z18.

3D CAD images of test specimens: (a) Tensile, (b) Bending, and (c) Compression.

The team studied seven infill patterns – catfill, diamond, hexagonal, Hilbert, linear, moroccocanstar, and sharkfill –  and infill densities of 25%, 30%, 40%, 50%, 70%, 90%, and 100%. Two shell layers were used for all samples, and the print bed temperature was between 23-70° for CFR-PLA, and 110°C for the three types of ABS material, to help reduce shrinkage and warping.

“At each test condition of all the types of tests (mechanical, rheological and thermal), 3 test specimens were prepared and tested, and then the average value was taken for the data analysis to improve the accuracy and reliability of the experimental data,” the team wrote.

Appearance of the printed compression test specimens: (a) PLA, (b) ABS, (c) CFR-PLA, (d) CFR-ABS, and (e) CNT-ABS.

First, the 3D printed samples underwent mechanical testing to determine tensile modulus, flexural modulus, and compression properties. Using differential scanning calorimetry (DSC), the researchers measured melting and crystallization behaviors in a liquid nitrogen atmosphere, and found “the volume fractions of the reinforcement and matrix of the composite filaments” with the help of thermal gravimetric analysis (TGA).

Appearance of printed tensile test specimens: (a) PLA, (b) ABS, (c) enlarged view of PLA, and (d) enlarged view of ABS.

Using a thermal imaging camera, they detected how much heat was released as the figure above was printed with 100% infill density, 20 mm/s infill speed, and 215°C set nozzle temperature. Finally, they used scanning electron microscopy (SEM) to observe and perform morphological testing on the surfaces of the 3D printed specimens that were broken during mechanical testing.

Infill density affects the strength of 3D printed parts. By increasing infill density, you then increase the tensile modulus and decrease porosity, which increases the “strength of the mechanical bonding between layers.”

Relationship between tensile modulus and infill density for PLA.

“For pure PLA, parts with 100% infill density obtained the highest Young’s modulus of 1538.05 MPa,” the researchers note.

But, structure gaps can occur more frequently with low infill densities, which reduces part strength. In the figure below, you can see “the changes in porosity of the structure with the infill density.”

3D printed specimens with infill densities: (a) 25% (b) 50% and (c) 100%.

“Of the tested infill speeds from 70 to 110 mm/s; 90 mm/s infill speed gave the highest Young’s modulus for pure PLA,” they wrote.

Print speeds over 90 mm/s could cause polymer filament to melt, and result in poor adhesion and lower strength. To avoid this, the print speed must be compatible with the set nozzle temperature, and an appropriate combination of speed and set nozzle temperature “can reduce the shrinkage of the parts being printed.”

Relationship between tensile modulus and infill speed for PLA.

3D printed PLA samples were tested with the different infill patterns at 50% infill density, 90 mm/s speed, and 215°C set nozzle temperature.

3D printed samples with infill patterns: (a) Linear, (b) Hexagonal, (c) Moroccanstar, (d) Catfill, (e) Sharkfill, (f) Diamond, and (g) Hilbert.

“Among these seven patterns, the linear pattern gave the highest tensile modulus of 990.5 MPa. This can be justified as the linear pattern should have the best layer arrangement (in terms of the bonding between the layers) with the lowest porous structure,” the team explained.

They found that the print temperature has “a significant effect on the tensile modulus.” 215°C provided the best tensile performance, as lower temperatures might cause poor melting, and thus weak bonding. The set nozzle temperature and print speed correlate, and “should be chosen carefully based on the material being used and the part geometry being printed.”

To study the effect on tensile properties, they were printed with the following parameters: 90 mm/s infill speed, linear pattern, 10% infill density, and 215°C set nozzle temperature for PLA, and 230°C for ABS. The researchers found that the tensile modulus of pure PLA (1538.05 MPa) was far higher than for pure ABS.

“In this study, CFR-PLA gave the largest tensile modulus of 2637.29 MPa while pure ABS (919.52 MPs) was the weakest in tensile strength,” they wrote.

Tensile modulus of the five printing materials.

Reinforcing ABS and PLA with fiber causes higher tensile modulus, though pure PLA was stronger than the CNT-ABS.

Even at 90° of bending, the PLA and ABS samples only had a small crack in the middle, and did not break.

3D printed specimen in bending test.

At 1253.62 MPa, the CFR-PLA had the highest bending modulus, while pure PLA was the lowest at 550.16 MPa.

During compression tests, none of the materials were crushed or broken, and pure ABS was found to be the toughest.

“As evident, pure PLA gave the highest compressive strength while the compressive modulus of CFR-PLA (1290.24 MPa) is slightly higher than that of pure PLA (1260.71 MPa) (higher gradient of the liner region). CFR-ABS and CNT-ABS follow the same trend but CNT-ABS is slightly tougher than CFR-ABS,” the team explained. “Pure ABS shows the lowest compressive strength and modulus (478.2 MPa) but shows the most ductile behavior of the five materials.”

Compressive stress-strain curves of test materials.

Finite element analysis (FEA) by ANSYS was used to visualize stress distribution for the tensile, bending, and compression testing of PLA.

Equivalent stress distribution for tensile test.

“The stress distribution shows that a uniform stress is created in the gauge length of the test piece,” they explained.

“Higher compressive loading will cause the material to have internal crack initiations thereby allowing the PLA to buckle excessively.”

The team concluded through DSC analysis that “the strength of the 3D printed samples is dependent upon the set printing parameters and the printing materials more than the crystallisation.” While the infill speeds differ, the glass transition temperature (Tg) of the samples were similar.

“In this study, cooling of 3D printed parts occurred naturally by releasing heat to the surroundings while printing without any control on the cooling rate,” they stated.

DSC curves of PLA parts printed at different set nozzle temperatures.

As expected, the set nozzle temperature did not significantly effect the Tg, and material crystallization at different temperatures didn’t really affect part strength. But, the tensile modulus did change with the temperature.

TGA was used to analyze the weight loss variation of the composite materials against increased print temperature.

TGA diagrams of short fiber-reinforced composite filaments.

“Degradation temperatures (Td) of these materials can be determined from the mid-point of the descending part of each curve, which is approximately 331.85 °C for PLA. This value showed some sort of agreement to the value reported in commercial PLA data sheets – 353 °C,” they wrote.

Pure PLA typically has a higher Young’s modulus than pure ABS, so it can help to add “a higher volume fraction of reinforcement into the ABS matrix.” Brittle CFR-PLA and CFR-ABS filaments could have their flexibility affected if more carbon fiber is added, which can cause filament feed issues.

Thermal image during 3D printing.

An infrared thermal camera was used to observe 3D printing. The yellow area is the brightest, and hottest: this is where the polymer was extruded from the nozzle. The color changes to orange where the material starts to solidify, and the “red, pink, purple, and blue areas are at lower temperatures, respectively.” The red circle marks the temperature at the printer wall – less than the sample actually being printed.

“SEM images showed that the strength of the printed samples was dependent upon the arrangement of their layers,” the team noted.

Normal and SEM images of fracture surfaces of PLA samples: (a) 25% and (b) 100% infill density.

Observing the fracture surfaces of broken PLA samples with SEM showed that “the air gaps of 25% infill density sample is larger than that of 100% infill density.”

Looking at infill speed with SEM, the team noted that “the best orderliness” comes from 90 mm/s infill speed.

Incompatibility between the material matrix and the reinforcement can cause porosity in the 3D printed samples, but the latter can “contribute in increasing the mechanical properties by bearing the load.” You can see below that the pure PLA has a more regular layer alignment when compared to pure ABS.

SEM images of 3D printed parts at 19X magnification: (a) PLA, (b) ABS, (c) CFR-PLA, (d) CFR-ABS, and (e) CNT-ABS.

CFR-ABS is more porous than CFR-PLA, and both are rougher than the materials in their pure forms.

“Meantime, CNT-ABS shows a better arrangement of individual layers than the other two carbon fibre reinforced materials and also than the pure ABS as well,” they explained.

The last SEM images compare the size of the carbon fiber and carbon nanotube reinforcements. The fracture surface of the CNT-ABS shows some small holes, “due to the embedded carbon nanotubes in the matrix.”

“Compared to the matrix-reinforcement compatibility, both materials show some sort of incompatibility by having cracks and voids between the fibre and matrix,” they wrote.

“On the other hand, although the overall strength of CNT-ABS is improved by CNT particles, the flexibility of this material was decreased compared to the pure ABS as CNT-ABS being more brittle.”

SEM images of fracture surfaces at 1.00 KX magnification: (a) CFR-PLA and (b) CNT-ABS.

They found that the optimal settings to improve the performance of the five 3D printing materials were 100% infill density, 90 mm/s infill speed, 215 °C of set nozzle temperature, and linear infill. Of the five materials, CFR-PLA had the strongest tension, bending, and compression, with the highest modulus.

Overall, it is obvious that the set printing parameters can significantly influence the mechanical properties of 3D printed parts. It can be claimed that the printing speed and set nozzle temperature should be matched to ensure proper melting of filaments and also to control the material solidification process,” the researchers concluded.

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Nanyang Technological University reviews use of carbon nanotubes in 3D printing

Researchers from the Singapore Centre for 3D Printing School of Mechanical and Aerospace Engineering Nanyang Technological University have published a review summarising research on carbon nanotubes (CNT) and their use in 3D printing. The research paper titled, Directed and On-Demand Alignment of Carbon Nanotube: A Review toward 3D Printing of Electronics, categorizes the alignment methods of carbon […]

Comparing FDM 3D Printed Parts with Carbon Nanotubes, Continuous Carbon Fiber and Short Carbon Fiber

Fused deposition modeling, or FDM, 3D printing has several advantages – thermoplastics can be used, which are easy to handle and are strong and durable enough to be used for producing both prototypes and practical parts. Additionally, FDM 3D printers use a simple mechanism to melt and extrude resin that doesn’t need expensive parts, like lasers, which makes the machines less expensive. But, the technology does not always provide enough strength for mechanical parts.

That’s why additional materials with good mechanical properties, such as carbon nanotubes (CNT) and fiber reinforced composites, are often added to improve strength; depending on the length, carbon fiber can also be divided up into both short and continuous fiber. A group of researchers from Doshisha University and Kyoraku Co., Ltd., both in Japan, recently published a study, titled “Comparison of strength of 3D printing objects using short fiber and continuous long fiber,” that compared the usefulness and strength of objects 3D printed with short carbon fiber, continuous carbon fiber, and multi-wall carbon nanotube (MWCNT).

The abstract reads, “In this research, composite materials were used to improve the strength of FDM 3D printed objects. The nanocomposites made from polylactic acid as matrix and multi-wall carbon nanotube as filler, short carbon fiber reinforced composite and continuous carbon fiber reinforced composite were prepared, and tensile test was carried out. As a result, the continuous fiber reinforced material exhibited tensile strength of about 7 times and elastic modulus about 5 times that of the other two materials. The strength was greatly improved by using the continuous fiber. The fracture surface after the test was observed using a scanning electron microscope. The result of observation shows that adhesion between the laminated layers and the relationship between the fiber and the matrix are bad, and improving these are necessary to increase strength. Comparing those materials, it is possible to improve the strength in some degree by using short fiber while maintaining ease of printing. On the other hand, by using continuous fiber it can be achieved significant strength improvement while printing was complicated.”

The fracture surface of PLA/MWCNT

To make their PLA/MWCNT nanocomposite, the researchers used polylactic material as a matrix, with MWCNT as a filler, and formed the material into a 1.75 mm filament. They used commercial ONYX, carbon fiber, and NYLON materials from Markforged to 3D print tensile test pieces from continuous carbon fiber reinforced thermoplastic (continuous CFRTP) and short carbon fiber reinforced thermoplastic (short CFRTP).

“The specimen shape is different due to the limitation by the performance of the 3D printer,” the researchers wrote in the paper. “For PLA/MWCNT, smaller one was chosen to avoid warp and print quickly. The PLA/MWCNT has three outer walls and fills inside alternately at 45 degrees and -45 degrees.”

For the continuous CFRTP, carbon fibers oriented in the load direction were 3D printed in the center, while the outside was covered with either neat resin or short fiber reinforced composite; this last was used to 3D print the short CFRTP in the same manner as the PLA composite had been fabricate.

The researchers completed a tensile test on the pieces, and used a scanning electron microscope to observe images of the specimen’s fracture surface. They also looked at their stress and strain.

“In PLA/MWCNT, the stress increased almost linearly until fracture,” the paper explained. “The breaking strain was about 1 ~ 2%, and no stress reduction was occurred. Compared with neat PLA, the elastic modulus was not greatly improved but the tensile strength was improved and increased by 48% when 1wt% of MWCNT is added. In that case, the tensile strength was 53 MPa and the Young’s modulus was 3 GPa. Until 1 wt%, the tensile strength was improved as more CNT is added, but strength was decreased when 3wt% was added. It is because the aggregation of MWCNT. The aggregations are considered to act as internal defects of the material.”

Aggregates and voids

When more MWCNT was added, the number of aggregates increased. The researchers found that the relationship between the fiber and the matrix, along with adhesion between the laminated layers, was not good – when these are improved, the strength will increase. Significant strength improvements can be achieved by using continuous fiber, but the 3D printing process is complicated, and it’s necessary to use modified equipment, such as a special nozzle. But short fiber is easier to print, and still offers some degree of improved strength.

“The short CFRTP and PLA/MWCNT are inferior in mechanical properties compared to the continuous. But they can be printed with conventional 3D printers without special modifying,” the researchers explained. “Especially the nanocomposites demonstrate its effect by adding a small amount. The mass concentration of fiber was 35.7 wt% for continuous CFRTP and 14.3 wt% for short CFRTP, but MWCNT was 3wt% or less. Generally, the smaller the amount of reinforcement, the more easy to print. In fact the PLA/MWCNT nanocomposite can be printed with commercially available 3D printer without special modified in this study. Continuous fiber and short fiber material should each have merits and demerits and should be used properly.”

The broken specimen (continuous CFRTP)

Co-authors of the paper are T. IsobeT. TanakaT. Nomura, and R. Yuasa.

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