Revealing The Process-Structure-Property Correlati
Revealing The Process-Structure-Property Correlati
https://doi.org/10.1007/s10443-024-10279-0
RESEARCH
Received: 19 July 2024 / Accepted: 1 October 2024 / Published online: 23 October 2024
© The Author(s), under exclusive licence to Springer Nature B.V. 2024
Abstract
This study employed a high-extrusion-rate Fused Deposition Modeling (HFDM) 3D print-
er, with the nozzle diameter enlarged from 0.4 mm to 1.0 mm. The increase in nozzle
diameter (from 0.4 mm to 1.0 mm) significantly enhanced the volumetric deposition rate,
thereby reducing the time required to print each layer and shortening the overall manu-
facturing cycle. In addition, the larger nozzle diameter increased the width and height of
each printed bead, which shortened the required path length per layer, further improving
printing efficiency. Short-carbon-fiber filled polyamide 12 (PA12-CF) is used as the test
material. The three-point bending test samples are prepared with the HFDM system, where
the effects of extrusion width and layer height, as printing parameters, on the flexural
properties are investigated. Furthermore, the fiber orientation within the deposited beads
is measured using optical microscopy and imaging process software ImageJ. Experimental
results indicate that with an increased layer height and extrusion width, PA12-CF samples
exhibit improved mechanical properties, where the bending strength and stiffness can be
increased up to ~ 20%, and ~ 30%, respectively. The fiber orientation angle measurements
indicate that with smaller values of layer height and extrusion width, the fibers tend to
align more parallel to the material extrusion direction. As these printing parameters in-
creased, the fibers tend to align more diversely to the transverse directions, which ulti-
mately benefits the increment of the flexural resistance of the entire samples. Additionally,
isothermal annealing process improves the bending strength and bending modulus of the
samples by approximately 12% and 13%, respectively.
Keywords High extrusion-rate FDM · Short carbon fiber filled polyamide · Three-point
bending test · Fiber orientation angle · Process-structure-property relation
Zhaogui Wang
[email protected]
1
Department of Mechanical Engineering, Naval Architecture and Ocean Engineering College,
Dalian Maritime University, Dalian, Liaoning 116026, China
2
Houston International Institute, Dalian Maritime University, Dalian, Liaoning 116026, China
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
494 Applied Composite Materials (2025) 32:493–523
1 Introduction
Fused Deposition Modeling (FDM) based Large Area Additive Manufacturing (LAAM),
also known as Big Area Additive Manufacturing (BAAM), has been a rapidly developing
additive manufacturing technology in recent years that focuses on the production of large
components and structural parts. LAAM (or BAAM) achieves efficient manufacturing of
complex shapes and large structures by layer-by-layer addition of material [1–3]. Com-
pared to traditional manufacturing methods, LAAM offers advantages such as high material
utilization, shorter production cycles, and greater flexibility [4, 5].The basic principle of
LAAM involves feeding the material into the print head through a feed system, where it
is heated and melted. The molten material is then extruded layer by layer through a nozzle
onto the build platform to form the desired part. Common materials used in HFDM include
thermoplastics, composites (fiber/polymer, etc.) [6]. Thermoplastic materials such as poly-
propylene (PP), polyamide (PA), and polycarbonate (PC) are used in the manufacture of
automotive parts and housings of industrial equipment [7]. Composite materials such as
carbon fiber reinforced composites are suitable for the production of large, lightweight, and
high-strength structural components. LAAM has significant application potential in fields
such as automotive manufacturing and construction engineering. In automotive manufactur-
ing, LAAM is used to produce body panels and chassis components, enabling rapid iteration
of product designs [2, 8]. In the construction engineering field, LAAM technology is used to
fabricate large building components, significantly reducing construction costs and time [9].
Improving printing efficiency is one of the core objectives of LAAM with high extrusion
rates. Current research mainly focuses on the following areas: optimizing heating systems
and extrusion control systems to further enhance material extrusion rates [10]. Some studies
have proposed improved screw-based extruders that can increase material flow while main-
taining stable temperatures, thereby achieving higher printing efficiency [11]. Parallel print-
ing with multiple nozzles is another method to enhance efficiency, significantly reducing the
manufacturing time of large components [12]. Additionally, using larger nozzle diameters
can increase material extrusion rates, thereby shortening print times [13]. However, larger
nozzle diameters may affect the print resolution and detail accuracy [14].Thus, maintain-
ing a balance between printing speed and high precision remains a key challenge. Existing
studies have proposed several methods to improve printing efficiency and strategies for
optimizing printing parameters, but there may be technical bottlenecks in practical applica-
tions, such as the trade-off between nozzle diameter and printing resolution, and the limited
efficiency improvements of the heating system.
Particularly, PA12-CF is a carbon fiber reinforced composite material based on polyam-
ide 12 (PA12), known for its excellent mechanical properties, low density, and good thermal
stability. It is widely used in aerospace, automotive manufacturing, and industrial equip-
ment sectors [15]. PA12-CF combines the low density and chemical resistance of PA12 with
the high strength and rigidity of carbon fibers, resulting in lightweight and robust composite
material [16, 17]. In the FDM process, PA12-CF is fed in the form of filaments into a heated
nozzle, where it is melted and extruded layer by layer to form complex three-dimensional
structures. PA12, which serving as the matrix material, offers excellent adhesion and work-
ability, ensuring robust interlayer bonding and overall structural stability during the form-
ing process. Carbon fibers, acting as the reinforcement, improve the material mechanical
properties of the material, particularly tensile strength and rigidity, allowing printed parts
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 495
to exhibit superior mechanical performance under load conditions [18–21]. The distribution
and orientation of carbon fibers significantly influence the performance of the final prod-
uct. By optimizing the distribution of carbon fibers within the PA12 matrix, it is possible
to effectively enhance the tensile strength, heat resistance, and dimensional stability of the
components [22–24]. In practical applications, PA12-CF manufactured through FDM tech-
nology produces lightweight, high-strength components that are widely used in the aero-
space, automotive, and industrial equipment sectors. Compared to traditional materials, the
use of PA12-CF in FDM not only improves manufacturing flexibility and efficiency, but
also reduces production costs. This highlights the significant potential and promising future
of additive manufacturing technology in the industry of high performance [18, 25]. With
the continuous advancement of FDM technology and the further optimization of PA12-CF
materials, this material is poised to find even broader applications in various fields in the
future. This trend is expected to drive innovation and development in the manufacturing
industry [26].
In large-area additive manufacturing (LAAM) with high extrusion rates, printing param-
eters such as build orientation, extrusion rate, layer height, extrusion width, nozzle tempera-
ture, and print speed significantly impact the mechanical properties of the final product. For
instance, build orientation plays a critical role in determining the performance of printed
parts. Due to the relatively weak interlayer bonding in vertically deposited layers, in-plane
deposition along the material loading direction typically exhibits superior mechanical
properties compared to the vertical direction. Other key factors affecting these properties
include raster gap, raster angle, layer thickness, and infill density. The combined influence
of these printing parameters on part performance was complex, making it crucial to evalu-
ate their synergistic effects to optimize the process for real-world manufacturing needs [27].
Studies had shown that the tensile and flexural strengths of ABS materials are significantly
reduced when oriented perpendicular to the deposition direction. Layer thickness and print
speed were also critical factors influencing the mechanical performance of ABS parts [28].
Research on build orientation had further indicated that samples printed along the Y-axis
exhibited the best tensile strength and the lowest production cost, while samples printed
along the X-axis demonstrated better flexural strength and moderate cost [29]. Rayegani et
al. used a full-factorial experimental design to study the effects of build orientation, raster
gap, raster angle, and extrusion width on tensile strength and identified an optimal process
combination to achieve maximum tensile strength [30]. Sood et al., using response surface
methodology (CCD) and analysis of variance (ANOVA), found that layer thickness and
raster angle had a much greater impact on residual stress and part deformation than other
controllable factors [31]. Mohamed et al., developed a mathematical model to predict pro-
cessing time, material cost, and mechanical performance, concluding that layer thickness,
raster gap, and build orientation were the most significant variables influencing these out-
comes [32]. Furthermore, Sood et al. studied the effects of printing parameters such as layer
thickness, build orientation, raster angle, raster width, and raster gap on the tensile, flexural,
and impact strengths of printed parts, and proposed important strategies for process optimi-
zation to improve the mechanical performance of materials in additive manufacturing [33].
Durgun et al. found that samples printed in the X and Y directions achieved higher strengths.
They also reported that flexural strength decreased with an increase in raster angle [34]. Liu
et al. investigated the effects of printing variables—orientation, layer thickness, raster angle,
raster width, and raster gap—on the mechanical properties (tensile, flexural, and impact
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
496 Applied Composite Materials (2025) 32:493–523
strengths) of PLA parts produced by FDM. Parts printed at a 0° raster angle in the X direc-
tion showed higher flexural strength [35]. While many studies have explored the impact of
individual printing parameters on performance, the complex interactions between multiple
parameters have not been fully investigated, such as how to maintain good fiber distribu-
tion and mechanical properties while increasing the extrusion rate. In addition, changes in
nozzle diameter affect the selection range of layer height and extrusion width. Fischer et
al. improved the porosity of samples by combining different nozzle diameters and layer
heights [36]. Larsson et al. studied the impact of increasing nozzle size in the FFF pro-
cess. Samples were produced using seven different nozzle sizes (ranging from the standard
0.4 mm to 2.0 mm), and the results indicated that as the nozzle diameter increased, the cor-
responding extrusion width also increased, leading to an 80% increase in productivity and
a 50% improvement in the strength of the printed parts [37]. Czyżewski et al. demonstrated
the importance of selecting an appropriate layer height based on the nozzle diameter. The
ratio of layer height to nozzle diameter should not exceed 0.8. When using a larger nozzle
diameter, maintaining a constant layer height at 0.2 mm can provide better conditions for
melting each subsequent layer during the contact of the hot extrudate with the previously
printed layer. This phenomenon likely has a decisive impact on the formation of interlayer
adhesion in the produced samples [38]. Aliheidari et al.‘s research shows that for a given
nozzle diameter and layer height, the layer width is controlled by the extrusion flow rate.
Technically, the layer width is limited to within approximately 30% of the nozzle diameter
[39]. Kuznetsov et al. studied the use of different nozzles (0.4, 0.6, and 0.8 mm) and a range
of layer heights from the machine’s minimum to maximum physical limits. For the samples
studied, the strength decreased by approximately 3.5 times as the layer height increased
from the minimum to the maximum [40].
Furthermore, fiber-reinforced composites consist of a matrix material and fiber reinforce-
ments, where the orientation of the fibers directly influences the overall performance of the
material [41–45]. Different fiber orientations can lead to varying mechanical properties of
materials under stress [46, 47]. Therefore, understanding the influence of fiber orientation
on mechanical performance is crucial for material design and applications. Fiber orientation
under different arrangements can affect shear strength, the addition of fibers has a minimal
impact on the shear strength of vertically printed samples. Typically, samples with fibers
arranged in a 0° orientation (horizontal printing) exhibited better shear performance com-
pared to those with fibers arranged in a 90° orientation [48]. When the fibers are aligned par-
allel to the loading direction, the materials can fully utilize the high-strength and modulus
properties of the fibers, significantly improving their tensile strength and stiffness [49, 50],
In tensile testing, when the fibers are aligned parallel to the loading direction, the strength
and modulus of the fibers can be maximized during the tensile process. This is because the
external load can be efficiently transmitted along the fiber direction, allowing the fiber’s
strength and stiffness to directly resist the load, significantly improving the tensile strength
and stiffness of the material. For example, in unidirectional fiber composite materials, the
tensile strength along the fiber direction can be several times higher than that of the matrix
material, resulting in excellent tensile performance under stress [51–53]. However, when
the fiber orientation is perpendicular to the tensile load direction, the tensile strength of
the material mainly relies on the matrix. In this case, the fibers do not enhance the tensile
strength, and since the matrix material is relatively weak, the overall tensile strength is low
[54–58]. Additionally, the orientation of the fibers also significantly affects the compres-
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 497
sive performance. When the fibers are aligned parallel to the direction of compressive load,
the material exhibits higher compressive strength and modulus. This is because the fibers
effectively resist compressive deformation along the axial direction, providing excellent
compressive properties [59, 60]. Further, the FDM-printed thermoplastics also exhibited
significant improvement on the flexural resistance performances owing to the addition of
carbon fiber reinforcements [61, 62]. In addition, in FDM processes, for a fixed nozzle
geometry and printing parameters, higher extrusion rates lead to an increase in bead width
compared to lower extrusion rates. Studies indicate that wider beads can provide stronger
interlayer interfaces, thus enhancing the ultimate tensile strength of the final product [63].
This strengthening effect is attributed to several factors, including an increase in the inter-
layer contact area and greater thermal mass. This prolongs the bonding time between layers
when both are above the glass transition temperature (Tg) [64, 65], as supported by research
[66].
We recently proposed a simply modified FDM 3D printer to achieve extended extrusion-
rate up to 100% higher as compared to desktop-size 3D printer (nozzle of 0.4 mm) [67],
which is referred as the High extrusion-rate FDM system. In the field of additive manufac-
tured fiber-reinforced composites, critical printing parameters such as printing layer height,
extrusion width, printing orientation, and infill direction have a significant impact on the
final product performance [68–70]. In this study, we evaluate the effects of printing param-
eters (i.e., layer height, and extrusion width) on the resulting mechanical properties of the
HFDM-produced composites. PA12-CF composite material is used as the test material. The
three-point bending test is chose as the representation of the mechanical performance indi-
cator of the HFDM products. To further explore the process-structure-property relations in
HFDM of short fibrous composites, the fiber orientation angles of the deposited composite
beads are measured via an optical microscopy approach. Additionally, the impact of iso-
thermal annealing treatment on the performance of HFDM-printed PA12-CF composites is
investigated.
Currently, various types of printers are used in FDM 3D printing research, with open-source
desktop 3D printers being particularly favored for their flexible printing modes, low cost,
and wide applications. However, open-source desktop printers are often limited by print
size, accuracy, and speed When it comes to printing large volumes and real-time supplied
prints, the 0.4 mm diameter nozzle’s extrusion rate becomes a bottleneck that restricts rapid
prototyping, resulting in prolonged printing times and low efficiency. This issue is particu-
larly pronounced when printing fully filled and slow-speed samples [38]. To address this
issue and improve the extrusion rate of molten materials in FDM 3D printers, this study
utilizes a custom nozzle with a diameter of 1.0 mm to increase the material extrusion rate.
This modification allows for the setting of larger layer heights and extrusion widths, thus
significantly reducing the number of G code execution cycles and shortening the forming
time for samples of different sizes, ultimately improving the efficiency and rapid production
capabilities of 3D printing [71, 72].
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
498 Applied Composite Materials (2025) 32:493–523
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 499
In this study, the ASTM D790 method is used to test the three-point bending samples. The
geometric structure of the 3D-printed samples is modeled using SolidWorks software. The
software export the models as .STL files, which are then imported into the 3D printing
slicing software. The main dimensions of the sample, the printed object, and the printing
orientation are shown in Fig. 2 [73], and the printing parameters are detailed in Table 2.
The experiment investigates the impact of the layer height and extrusion width param-
eters on the bending performance of HFDM-printed PA12-CF material samples. Initially,
under a layer height of 0.4 mm, the effects of different extrusion widths (1.0 mm, 1.5 mm,
2.0 mm) are tested, with 10 samples printed for each width, half of which are treated with
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
500 Applied Composite Materials (2025) 32:493–523
an isothermal post annealing process (to enhance the mechanical properties). Subsequently,
under a fixed extrusion width of 1.0 mm, the effects of different layer heights (0.4 mm,
0.533 mm, 0.8 mm) are studied, with 10 samples printed, and half of which are annealed.
Tables 3 and 4 present the detail of experimental printing parameters setup. In addition, a
5 mm slicing distance around the sample is set using PrusaSlicer software to ensure stability
during printing and uniformity of material extrusion.
During the FDM printing process, temperature variations between layers and the introduc-
tion of carbon fibers can induce internal stresses within the material. To eliminate these
stresses, improve crystallinity, and enhance dimensional and mechanical properties, we
conduct an isothermal annealing treatment on the printed samples. The annealing process is
performed in a TATUNG-TLD050 (Shibei instruments Inc., Shanghai, China) convection
oven, initially ramping up at a rate of 5 °C/min to 80 °C, holding for 2 min, followed by
constant temperature annealing at 80 °C for 6 h, and finally cooling down at 3 °C/min to
room temperature (20 °C), as did in a previous related study [74, 75]. Throughout the cool-
ing process, the oven remains closed to ensure that the samples cool gradually. The convec-
tion oven circulates heated air, allowing it to flow evenly around the samples and providing
a 360° heat source [76, 77]. Compared to traditional gas or electric ovens, convection ovens
distribute heat more uniformly, leading to more consistent heating results [78, 79].
The three-point bending test of the samples prepared by HFDM process is conducted using
the CTM-8010 microelectronic universal material testing machine (Xieqiang Instrument
Manufacturing Co., Ltd., Shanghai, China). To ensure consistency and reliability during the
testing process, the samples were clamped. This step prevents sample displacement, reduces
testing errors, ensures uniform load distribution, and the tests were conducted at a constant
loading rate of 2 mm/min, the test diagram is shown in Fig. 3. The PA12-CF samples are
tested using the DSC-500 C differential scanning calorimeter (Jiezhun Instrument Equip-
ment Co., Ltd., Shanghai China) to determine the peak temperature and enthalpy character-
istics of the test. Thermogravimetric analysis (TGA) is a technique that studies the thermal
stability, composition, and decomposition characteristics of a sample by measuring its mass
change during a controlled heating process. Thermogravimetric analysis is performed on
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 501
Fig. 4 Bending performance of PA12-CF samples with different printing layer heights
The bending strength is a critical indicator of a material’s ability to resist failure under
bending forces. In this study, we observe significant variations in the bending strength
with changes in the height of the printing layer. According to the bending strength analysis
shown in Fig. 4(a), the sample exhibits a bending strength of 70.5 MPa at a layer height of
0.4 mm. This result indicates that the PA12 material containing short carbon fibers demon-
strates a greater bending strength at lower layer heights [15]. As the layer height increases to
0.533 mm, the bending decreases slightly to 69.1 MPa. This change due to the influence of
layer height on the distribution and alignment of carbon fibers at higher settings, potentially
leading to stress concentration and failure under load. According to previous research [80],
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
502 Applied Composite Materials (2025) 32:493–523
when the layer height is smaller (such as 0.4 mm and 0.533 mm), lower layer heights typi-
cally exhibit higher bending strength. This is because at lower layer heights, the bonding
strength between layers is stronger. In this case, the interlayer bonding is tighter, leading
to greater adhesion. Additionally, lower layer heights require higher extrusion pressure for
effective deposition. This higher extrusion pressure resulting from the reduced layer height
ensures good contact between layers, ultimately enhancing the bonding strength. It is note-
worthy that the study by Dev et al. indicates that the bending strength consistently increases
as the layer thickness decreases [81]. In contrast, our research found that when the layer
height increases from 0.4 mm to 0.533 mm, the bending strength slightly decreases, but it
recovers and increases to 75.3 MPa at a layer height of 0.8 mm. This trend suggests that,
due to the specific printing parameters and material composition, an appropriate increase in
layer height can sometimes enhance the bending strength of the printed products.
The bending elastic modulus is an indicator reflecting a material’s ability to resist bend-
ing deformation within its elastic range,. In this study, we observe variations in the bending
elastic modulus with changes in the height of the printing layer. According to the analysis
of the bending elastic modulus shown in Fig. 4(b), at a layer height of 0.4 mm, the sample
exhibits a bending elastic modulus of 1.96 GPa. As the layer height increases to 0.533 mm,
the bending elastic modulus decreases slightly to 1.92 GPa. This change indicate that the
elastic performance of the material is somewhat affected at higher layer heights. However,
when the layer height increases further to 0.8 mm, the bending elastic modulus rises again to
2.06 GPa. This trend related to the distribution and arrangement of carbon fibers within the
material; an appropriate layer height could facilitate the formation of a more uniform and
effective reinforcement network, thereby enhancing the material’s bending elastic modulus.
As the layer height increases, the bending strength and bending elastic modulus of PA12-
CF change due to the effects of inter-layer and intra-layer bonding [82]. Compared to the
variations in bending strength and bending elastic modulus of samples with smaller layer
heights (0.4 mm and 0.533 mm), the sample with a layer height of 0.8 mm achieves the
highest strength. For layer heights of 0.4 mm and 0.533 mm, additional layers are needed
to bond with each other to achieve the desired total layer height. As the layer thickness
increases, the number of layers decreases [83]. This bonding is imperfect, as it only relies
on mechanical adhesion [82]. Therefore, the highest bending strength and bending elastic
modulus are observed with a layer thickness of 0.8 mm, which is consistent with previous
research findings [84].
Flexural deflection is another indicator that presents the resistance of a material to frac-
ture when subjected to bending forces. In this study, we observe significant differences in
flexural deflection with changes in the height of the printing layer. As indicated by the analy-
sis of the flexural deflection in Fig. 4(c), at a layer height of 0.4 mm, the sample exhibits the
maximum flexural deflection of 27.4 mm. As the layer height increases to 0.533 mm and
0.8 mm, the flexural deflection gradually decreases to 26.5 mm and 23.8 mm, respectively.
This trend suggests that as the layer height increases, the sample is more prone to fracture
under bending forces. This could be due to less tight interlayer bonding during the printing
process at higher layer heights, leading to an increased likelihood of cracks and fractures
in the material under stress [36]. Furthermore, as the layer height increases, the effect of
fracture deflection on the sample becomes smaller [85].
This section discusses the effect of printing layer height on the mechanical properties
of PA12 short carbon fiber reinforced material. Through experimental analysis of bending
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 503
strength, bending elastic modulus, and flexural deflection, the study reveals the significant
influence of layer height on material performance. Overall, the results demonstrate the con-
siderable impact of layer height on the mechanical properties of PA12 short carbon fiber
reinforced materials. At lower layer heights, both bending strength and elastic modulus
are higher, but this is also accompanied by greater flexural deflection and increased risk of
brittle fracture. However, with a proper increase in layer height, the mechanical properties
are optimized. Specifically, at a layer height of 0.8 mm, the material exhibits the highest
bending strength and elastic modulus, while flexural deflection decreases. These findings
emphasize the importance of optimizing layer height in additive manufacturing based on
material performance requirements, in order to balance the formation of reinforcement net-
works and interlayer bonding quality.
On the other hand, the impacts of different extrusion widths in PA12-CF samples are
depicted in Fig. 5. As shown in Fig. 5(a), the analysis of the bending strength indicates
that at an extrusion width of 1.0 mm, the sample exhibits a bending strength of 70.5 MPa.
With an increase in extrusion width to 1.5 mm, the bending strength increases to 75.2 MPa.
Further increasing the extrusion width to 2.0 mm results in the highest bending strength of
83.9 MPa. The bending strength increases as the raster width increases. With larger extrusion
widths, the freshly printed filament retains more thermal mass, resulting in slower cooling
and remaining above the glass transition temperature for a longer duration. This improves
the bonding between adjacent rasters, leading to higher bond strength. Additionally, the
larger the raster width, the greater the interlayer contact area, which further enhances the
adhesion strength [80]. Additionally, the variation in standard deviation also reflects the
influence of extrusion width on the stability of the bending strength. As the extrusion width
increases, the standard deviation gradually decreases, indicating improved stability in the
bending strength of the samples. This further underscores the importance of selecting an
appropriate extrusion width to optimize the bending performance of the material. Similar to
previous research conclusions, smaller extrusion widths can provide higher accuracy, while
an increase in extrusion width improves bending performance [86]. Excessive extrusion
width can lead to path gaps and reduced printing performance, while also increasing surface
roughness. Conversely, when the path width is set too small, it may cause overlapping and
further increase surface roughness [87].
The analysis of the bending elastic modulus in Fig. 5(b) shows that at an extrusion width
of 1.0 mm, the sample has a bending elastic modulus of 1.957 GPa. With an increase in
Fig. 5 Bending performance of PA12-CF samples printed with different extrusion widths
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
504 Applied Composite Materials (2025) 32:493–523
the extrusion width to 1.5 and 2.0 mm, the bending elastic modulus increases to 2.17 and
2.52 GPa, respectively. This trend indicates that increasing the width of the extrusion helps
to improve the bending elastic modulus of PA12 material containing short carbon fibers.
This enhancement is likely due to a more uniform distribution of carbon fibers within the
material as the extrusion width increases, forming a more effective reinforcement structure
and thereby improving the material’s resistance to bending deformation. Additionally, the
decrease in standard deviation also suggests that increasing the extrusion width improves
the stability of the bending elastic modulus of the samples. These results provide theoreti-
cal support for selecting an appropriate extrusion width in practical production scenarios.
Additionally, the fracture deflection analysis in Fig. 5(c) indicates that at an extrusion width
of 1.0 mm, the sample has the maximum fracture deflection of 27.42 mm. As the extrusion
width increases to 1.5 and 2.0 mm, the fracture deflection gradually decreases to 26.2 and
24.9 mm, respectively. This trend suggests that increasing the width of the extrusion cause
samples to be more prone to fracture under bending loads. This could be due to changes
in internal stress distribution within the material at higher extrusion widths, resulting in
increased susceptibility to cracking and fracture under bending stress.
This section discusses the effect of extrusion width on the mechanical properties of PA12
short carbon fiber-reinforced material. Through experimental analysis of bending strength,
bending elastic modulus, and fracture deflection, the study shows that extrusion width sig-
nificantly impacts the material’s mechanical properties. Overall, the results indicate that
increasing the extrusion width can effectively improve the mechanical performance of the
material. At smaller extrusion widths, the material exhibits lower bending strength and elas-
tic modulus, along with a larger fracture deflection, indicating a higher susceptibility to frac-
ture under stress. However, as the extrusion width increases, the bending strength and elastic
modulus of the material improve significantly, while the fracture deflection decreases. At an
extrusion width of 2.0 mm, the material demonstrates optimal mechanical performance.
In order to investigate the effect of fracture mechanisms on the bending strength and bend-
ing modulus of elasticity of the specimens, we further analyzed the macro-structure of the
fracture morphology of failed specimens under bending load. As shown in Figs. 6 and 7,
the surface structure of the failed specimens was observed from the side view and top view
using a Dino-lite (AnMo Electronics Corp., Taiwan, China) handheld microscope. For the
structural analysis of specimens with different layer heights, it can be observed that in the
unannealed specimens, due to the uneven distribution of internal stresses in the material
under load, cracks are more to propagate along specific directions, resulting in the failure
region being concentrated in the middle of the bent Sect. [80]; In contrast, the annealed
specimens exhibited improved material uniformity and ductility due to the release of inter-
nal stresses [88], which result in better crack resistance under the same loading conditions,
with the cracks being more widely distributed and the fracture regions smaller [53]. As the
layer height increases, the thickness and overall structural stiffness of the specimens are
enhanced. However, due to the increased number of inter-layer interfaces, stress concentra-
tion become more pronounced [89], particularly in positions where the loading direction is
parallel to the layered structure. Both the non-annealed and annealed specimens fractured
suddenly when reaching the load limit, which is consistent with previous research findings
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 505
Fig. 6 Macro-structure of failed bending specimens for various layer height. (a) 0.4 mm unannealed
sample, (b) 0.4 mm annealed sample, (c) 0.533 mm unannealed sample, (d) 0.533 mm annealed sample,
(e) 0.8 mm unannealed sample, (f) 0.8 mm annealed sample
Fig. 7 Macro-structure of failed bending specimens for various extrusion width. (a) 1.0 mm unannealed
sample, (b) 1.0 mm annealed sample, (c) 1.5 mm unannealed sample, (d) 1.5 mm annealed sample, (e)
2.0 mm unannealed sample, (f) 2.0 mm annealed sample
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
506 Applied Composite Materials (2025) 32:493–523
on the carbon fiber fracture mechanism [90]. The side and bottom surfaces shown in the
figures indicate the location and morphology of the fractures. From these images, the initia-
tion points, propagation paths of cracks, and the effect of different layer heights and heat
treatments on the bending strength can be further analyzed.
From the analysis of unannealed specimens, it can be concluded that due to the smaller
extrusion width, the bonding interfaces between layers are relatively few, and the stress is
more evenly transmitted. However, the unannealed material is more prone to fracture at
stress concentration points due to internal stresses. As the extrusion width increases, the
layered structure of the specimen becomes more prominent, with more bonding interfaces
between layers, leading to an increase in stress concentration areas [89, 91]. With wider
extrusion widths, cracks are more likely to propagate along the interlayer interfaces, making
bending fractures more noticeable. After annealing, for smaller extrusion widths, the speci-
men structure becomes denser, and its crack resistance under bending is enhanced. Cracks
tend to concentrate in specific areas, but the fracture toughness is better. As the extrusion
width increases, the annealed specimens exhibit better fracture resistance under loading.
Even though the number of interlayer bonding interfaces increases, annealing strengthens
the overall bonding of the structure, making the specimen less prone to interlayer fractures
during bending. The annealed specimens, due to the release of internal stresses from heat
treatment, show greater toughness and fracture ductility. It can be observed that under the
same loading conditions, the cracks in annealed specimens are more dispersed, and the
fracture areas are relatively smaller. This is because annealing improves the uniformity of
the material structure and tightens the bonding between layers, thereby reducing local stress
concentrations [78, 92]. From the images, the fracture characteristics of specimens with
different extrusion widths can be observed on the side and bottom surfaces. Cracks in unan-
nealed specimens are concentrated in the loading area, while annealed specimens exhibit a
more even stress distribution, with relatively smoother crack patterns.
In order to further analyze the effect of carbon fiber orientation on the bending strength
of PA12-CF at different layer heights and extrusion widths, a Keyence VHX-7000 optical
microscope is used to examine the distribution of carbon fiber orientation. As shown in
Fig. 8, cross-sections parallel to the Y and Z directions are selected and then cut, followed
by polishing the cross-sections in a polishing machine. The preparation steps for the metal-
lographic samples are as follows: first, the samples are embedded using metallographic
mounting powder, then the embedded samples are sanded with sandpaper, and finally, the
Fig. 8 Schematic diagram of the
cut surface
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 507
samples are polished with diamond paste to achieve a mirror finish on fabric. The grinding
and polishing process is carried out on metallographic sandpaper and polishing cloth, mini-
mizing sample deformation and maintaining the integrity of the cross-Sect. [93].
First, a comparison is made between the set values and actual measurements of the layer
height and extrusion width. Figure 9 presents the measured results of layer height and extru-
sion width for the printed samples. The maximum number of deposition beads observable
within the field of view is selected. For a theoretical layer height of 0.4 mm, the average of
six actual measurements is approximately 0.3965 mm, resulting in a relative error of about
0.875%. This indicates a difference of approximately 0.875% between the actual extru-
sion width and the theoretical value. The standard deviation of the actual measurements is
approximately 0.0075 mm, suggesting minimal dispersion among the six measurements and
relative stability of the data. This indicates consistent printing performance during extru-
sion, albeit with minor fluctuations. Similar methods are applied to calculate the actual
measurement results for other slicing parameters, as shown in Tables 5 and 6.
Next, we observe and analyze the influence of layer height on carbon fiber orientation.
We use the Keyence VHX-7000 optical microscope with the Opt-SEM (differential interfer-
ence contrast) illumination mode to observe the fibers. Fiber orientation is observed on the
polished surface of the samples using a 500× magnification lens, as shown in Fig. 10.
In this section, we study the relationship between layer height and planar fiber orienta-
tion distribution. Taking the molded samples with a layer height of 0.4 mm as an example,
we measure the planar fiber orientation angles of carbon fibers under 500× magnification.
The planar fiber orientation distribution (PFOD), also known as surface fiber orientation,
is determined by measuring the angle of the fibers relative to the printing direction of the
extruded filament on the polished surface of the samples, denoted as θ in the Figures.
ImageJ software is used to annotate the planar fiber orientation angles, as illustrated in
Fig. 9 (a) Comparison of slice setting values and actual measurements of layer height for 0.4 mm, (b)
Comparison of slice setting values and actual measurements of layer height for 0.533 mm, (c) Compari-
son of slice setting values and actual measurements of layer height for 0.8 mm, (d) Comparison of slice
setting values and actual measurements of extrusion width for 1.0 mm, (e) Comparison of slice setting
values and actual measurements of extrusion width for 1.5 mm, (f) Comparison of slice setting values and
actual measurements of extrusion width for 2.0 mm
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
508 Applied Composite Materials (2025) 32:493–523
Table 5 Comparison of the slice Slice Measurement value Average Relative Stan-
and measurement values of value (µm) value error dard
PA12-CF samples with different (mm) (µm) deviation
layer heights (mm)
0.4 393/386/411/394/398/397 396.5 0.875% 0.0075
0.533 526/517/509/505 514.25 3.518% 0.008
0.8 797/799/803 799.67 0.041% 0.0025
Table 6 Comparison of the slice Slice Measurement value Aver- Relative Stan-
and measurement values of value (µm) age error dard
PA12-CF samples with different (mm) value deviation
extrusion widths (µm) (mm)
1.0 984/913/979/992/1004 974.4 2.56% 0.0318
1.5 1494/1480 1487 0.867% 0.007
2.0 1970/1972 1971 1.45% 0.001
Fig. 10 Observation of short carbon fiber on PA12-CF printed samples with different layer heights, 500×.
(a) 0.4 mm layer height, (b) 0.533 mm layer height, (c) 0.8 mm layer height
Fig. 11. Through ImageJ, the first step is to import the microscopic image of the polished
surface of the sample. To better highlight the fiber orientation, the image is preprocessed by
enhancing the contrast. Next, the angle measurement tool is used to mark the printing direc-
tion of the extruded filament and the fiber orientation. Multiple measurements are taken at
different positions on the sample to determine the fiber orientation angles, and all angle data
is recorded using ImageJ software. Finally, the distribution of these angles is calculated to
determine the PFOD. We measure all visible fibers, resulting in a total of 50 fiber orientation
angle measurements, as shown in Table 7. For fiber orientation observations at layer heights
of 0.533 mm and 0.8 mm, we follow the same procedure shown in Fig. 11 (layer height
0.4 mm) to measure the planar fiber orientation angles, each obtaining 50 measurements,
respectively, for short carbon fibers.
When investigating the effect of layer height on the orientation angle of short carbon
fibers, we observe significant changes in the distribution of orientation angles, as depicted
in Fig. 12 (based on data appearing in Table 7) and Table 8. At a layer height of 0.4 mm,
most fibers (73.5%) have orientation angles concentrated within the range of 0° to 5°, with a
low average orientation angle (3.91°). This suggests a relatively orderly fiber arrangement,
possibly due to higher shear forces generated even at lower layer heights, which promote
higher fiber orientation. As the layer height increases to 0.533 mm, although the proportion
of fibers within the 0° to 5° range decreases (to 67.3%), there is an increase in the propor-
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 509
Table 7 The plane orientation angle of the carbon fiber in the sample with a layer height of 0.4 mm
Fiber Fiber Fiber Fiber Fiber Fiber Fiber Fiber
number orientation number orientation number orientation number orientation
1 0.631 14 6.245 27 1.757 40 0.524
2 0.921 15 8.868 28 10.394 41 6.829
3 4.139 16 5.412 29 6.868 42 4.991
4 2.08 17 3.475 30 3.607 43 1.532
5 3.734 18 3.873 31 11.821 44 9.402
6 1.83 19 2.635 32 2.072 45 4.357
7 4.054 20 2.11 33 4.619 46 2.19
8 3.013 21 0.599 34 4.289 47 0.685
9 0.654 22 4.627 35 0.531 48 1.874
10 1.663 23 6.762 36 1.125 49 1.239
11 0.854 24 1.833 37 3.138 50 1.658
12 2.37 25 11.443 38 6.293
13 5.534 26 3.127 39 8.854
Fig. 12 The arrangement of PFOD for samples with different layer heights. (a) 0.4 mm, (b) 0.533 mm,
(c) 0.8 mm
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
510 Applied Composite Materials (2025) 32:493–523
Table 8 Distribution characteristics of the fiber orientation angle in the plane of layer height
Layer 0°~5° 5°~10° >10° Mean planar fiber standard devia- variance of
heights orientation angle tion of planar fiber planar fiber
(mm) (°) orientation angle orientation
angle
0.4 73.5% 20.4% 6.1% 3.91 2.96 8.78
0.533 67.3% 29.1% 3.6% 4.39 3.5 12.25
0.8 37.7% 35.9% 26.4% 8.61 9.14 93.48
Fig. 13 The measurement results of short carbon fibers, arranged in different ways at various layer heights
tion within the 5° to 10° range, and the overall average orientation angle increases slightly
(to 4.39°). This indicates a beginning of slightly more scattered fiber alignment. At a layer
height of 0.8 mm, the proportion of fibers within the 0° to 5° range decreases significantly
(to 37.7%), while those exceeding 10° increase substantially (to 26.4%), resulting in a sig-
nificant increase in the average orientation angle (8.61°). This demonstrates that with a
further increase in layer height, the fiber arrangement becomes more disorderly and the
distribution of orientation angles becomes more dispersed. This trend of change is reflected
not only in the proportion of orientation angle distributions, but also in the increase in the
average, standard deviation, and variance of orientation angles, further confirming the sig-
nificant impact of layer height on the orientation angles of short carbon fibers.
Furthermore, to visually illustrate the distribution range and trends of planar fiber ori-
entation angles, the measurement results of short carbon fibers under different parameters
are arranged in columns for comparison using data histograms and the probability density
functions of Normal distribution (formula 1) and Weibull distribution (formula 2). The fitted
parameters and results are shown in Table 9; Fig. 13, comparing the distribution of short car-
bon fiber orientation angles at different layer heights. We draw the following conclusions:
with increasing layer height, the distribution of orientation angles becomes more dispersed,
indicating a decrease in the uniformity of fiber alignment. This change not only affects the
average orientation angle of the fibers, but also results in a significant increase in standard
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 511
Fig. 14 Observation of short carbon fibers in PA12-CF printed samples with different extrusion widths,
500×. (a) 1.0 mm extrusion width, (b) 1.5 mm extrusion width, (c) 2.0 mm extrusion width
Fig. 15 The arrangement of PFOD for samples with different extrusion widths. extrusion widths. (a)
1 mm, (b) 1.5 mm, (c) 2 mm
1 (x−µ)2
−
f (x; µ, σ) = √ e 2σ 2 (1)
2πσ 2
k x k−1 −( x )k
f (x; λ, k) = e λ (2)
λ λ
Furthermore, this section observes and analyzes the impact of different extrusion widths on
the orientation of carbon fibers. Figure 14 shows the orientation distribution of short carbon
fibers in PA12-CF samples with various extrusion widths. Figure 15 presents the scatter
plots of planar fiber orientation angles measured under different extrusion widths, while
Table 10 provides detailed descriptions of angle ranges, standard deviation, and variance.
Similarly, the measurement results of short carbon fibers under different extrusion widths
are arranged in columns for comparison using data histograms and the probability density
functions of normal distribution and Weibull distribution. The fitted parameters and results
are shown in Table 11; Fig. 16. As the extrusion width increases, there is a noticeable trend
of dispersion in the distribution of planar fiber orientation angles. Under smaller extru-
sion widths, the fibers tend to align closely along the direction approaching 0°~5°, with
a high proportion of fibers oriented at 73.5%. This high uniformity in orientation attrib-
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
512 Applied Composite Materials (2025) 32:493–523
Table 10 Distribution characteristics of the fiber orientation angle in the extrusion width
Extrusion 0°~5° 5°~10° >10° Mean planar fiber standard devia- variance of
width orientation angle tion of planar fiber planar fiber
(mm) (°) orientation angle orientation
angle
0.4 73.5% 20.4% 6.1% 3.91 2.96 8.78
1.5 58.3% 27.1% 14.6% 5.34 5.09 25.87
2.0 22.5% 40.8% 36.7% 9.63 6.25 39.04
Table 11 Parameters of the fitted Extrusion width (mm) Normal distribution Weibull
PDFs with different extrusion distribution
widths
μ σ k λ
1.0 3.831 3.014 3.919 1.079
1.5 5.692 5.377 5.614 0.963
2.0 9.525 6.290 10.645 1.592
Fig. 16 The measurement results of short carbon fibers, arranged in different ways at various extrusion
widths
uted to the restriction imposed by smaller extrusion widths on the freedom and randomness
of the fibers during printing, facilitating a more concentrated and directional alignment.
When the extrusion width is increased to 1.5 mm, the scatter plots of the measured planar
fiber orientation angles and data analysis show a change in the distribution of the planar
fiber orientation. The proportion of fibers in the 0°~5° range decreases from 73.5 to 58.3%
(a decrease of 15.2%), while fibers oriented between 5°~10° increase by 6.7% and 8.5%,
respectively (compared to the extrusion width of 1.0 mm). The mean, standard deviation,
and variance of the planar fiber orientation angles increase from 3.91, 2.96, and 8.78 to 5.34,
5.09, and 25.87, respectively. This indicates that with increasing extrusion width, fiber ori-
entation begins to exhibit greater dispersion, no longer approaching uniformity as observed
at 1.0 mm width. Finally, at an extrusion width of 2.0 mm, the scatter plots of the planar fiber
orientation angles measured indicate a more scattered overall distribution of the planar fiber
orientation. This suggests that with larger extrusion widths, fiber orientation becomes more
diverse without a pronounced centralized trend. This could lead to increased complexity and
deformation in fiber alignment during printing, making fiber orientation more unpredictable
and challenging to control. These findings are consistent with previous studies on the effect
of extrusion width on planar fiber orientation [94]. Additionally, single-factor analysis of
variance (ANOVA) indicates significant differences in the variance of the planar fiber ori-
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 513
entation distribution with changing extrusion width. The variance increases from 8.78 to
39.04 (a growth of 344.65%) as the extrusion width increases from 1.0 mm to 2.0 mm, sug-
gesting a wider and more uniform distribution of planar fiber orientation angles and reduced
uniformity in fiber alignment.
In conclusion, there are significant differences in the orientation angles of the planar
fibers under different extrusion widths, as illustrated in Fig. 17. With wider extrusions, the
lateral flow of polymer fluid towards the printing direction result in a more transverse orien-
tation of the encapsulated carbon fibers (less orderly alignment in the printing direction). On
the contrary, narrower extrusions tend to align fibers more along the flow direction. These
variations likely stem from the influence of extrusion width on the forces, deformation, and
arrangement of fibers during printing. Therefore, adjusting the extrusion width during 3D
printing offers effective control over the orientation angles of the planar fiber to meet diverse
application requirements. Research findings on fiber orientation with respect to layer height
and extrusion width suggest that extrusion width has a greater impact on fiber orientation
than layer height, consistent with previous studies [95]. Hence, it is recommended that,
compared to layer height, extrusion width is a more suitable parameter for altering fiber
orientation.
Different methods are studied to improve the mechanical properties of composite materials
in FDM 3D printing through various physical mechanisms. Post-manufacturing heat treat-
ments, such as annealing, improve the mechanical properties of 3D printed composite mate-
rials [96, 97]. Annealing under controlled environmental pressure strengthens the interface
bond between deposited beads, thereby increasing strength and modulus [98, 99]. Samples
with different layer heights and extrusion widths are separately subjected to annealing post-
processing, with results depicted in Figs. 18 and 19. For instance, comparing annealed and
non-annealed samples with a layer height of 0.4 mm, the bending strength significantly
increases from 70.5 MPa to 90.0 MPa after annealing. This significant improvement can be
attributed to the release of internal stresses within the material and the optimization of short
carbon fiber alignment during the annealing process [99]. Annealing helps alleviate residual
stresses generated during printing, leading to a more uniform and stable material structure
[100]. Furthermore, the bending elastic modulus of the samples increases from 2.0 GPa to
2.4 GPa after annealing. This change also reflects the impact of annealing on the internal
structure of the material. As a result of the increase in crystallinity, the polymer molecular
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
514 Applied Composite Materials (2025) 32:493–523
Fig. 18 The bending performance before and after annealing for samples with different layer heights. (a)
Bending strength, (b) Bending Elastic Modulus, (c) Fracture Deflection
Fig. 19 The bending performance before and after annealing for samples with different extrusion widths.
(a) Bending strength, (b) Bending Elastic Modulus, (c) Fracture Deflection
chains are arranged in an orderly. Moreover, annealing can also improve the interface bond-
ing between the carbon fibers and the matrix, allowing the carbon fibers to better reinforce
the material under bending loads [101–103]. Finally, the fracture deflection of the samples
decreases significantly from 27.4 mm to 9.4 mm after annealing. This change indicates
that while annealing enhances the bending strength and elastic modulus of the material,
it reduces its ability to resist fracture. This is because adjustment of the material’s inter-
nal structure during annealing can increase brittleness. Although annealing optimizes fiber
alignment and enhances crystallinity, it can also make the material more brittle in certain
directions, making it more prone to fracture under bending loads. For other layer heights and
extrusion widths of the samples before and after annealing, the trends in bending strength,
bending elastic modulus, and fracture deflection follow the results of the analysis for the
layer height of 0.4 mm.
Additionally, we have provided the stress-strain curves for PA12-CF samples before
and after annealing at different layer heights and extrusion widths, as shown in Figs. 20
and 21. From the curves, it can be observed that, regardless of layer height or extrusion
width, annealing significantly increased the maximum stress (i.e., peak strength) of the
samples. The purpose of annealing is to eliminate internal stresses and improve the crystal-
line structure of the material, thereby enhancing its mechanical properties. We can see that
the annealed samples exhibit higher stress at the same strain level, indicating better load-
bearing capacity. The stress of the unannealed samples is significantly lower than that of
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 515
the annealed samples, suggesting that the unannealed samples have higher residual stress or
incomplete crystalline structures, leading to inferior mechanical performance.
To investigate the effect of annealing on the thermal properties of PA12-CF samples,
samples are extracted from samples with a layer height of 0.4 mm and an extrusion width of
1.0 mm, following the procedures outlined in Sect. 2.3. Each sample is taken from annealed
and unannealed samples. The samples are weighed using an electronic balance (ATX124R,
Shimadzu, Japan) to ensure a sample mass between 5 and 10 mg. Crystallinity analysis of
the PA12-CF material is carried out using Differential Scanning Calorimetry (DSC). The
DSC analysis is performed at a heating rate of 10 °C/min from 20 °C to 300 °C, with 30 min
of nitrogen purging before the tests to prevent oxidation, and the nitrogen gas flow at 50 ml/
min during the tests. Figure 22 illustrates the DSC curves of PA12-CF samples before and
after annealing.
Based on processed DSC data and plotted using formula 3 [104], the crystallinity of
PA12-CF before and after annealing is calculated. In formula 3, ∆ Hm represents the melt-
ing enthalpy change of PA12-CF, and ∆ Hm ∗
denotes the melting enthalpy change when
fully crystallized. The ∆ Hm for PA12-CF is approximately 95 J/g [105]. Given the rela-
∗
tively low addition of carbon fibers (10 wt%), its impact on the melting enthalpy change is
assumed to be minor. The crystallinity of PA12-CF samples before and after annealing is
found to be 23.5% and 24.4%, respectively. These results indicate that annealing has a mini-
mal effect on the crystallinity of PA12-CF, likely due to its inherent stable crystallization
behavior as a composite material [106]. The inclusion of carbon fibers influence the crystal-
lization process, but if the fibers are uniformly dispersed and have an appropriate content,
their effect on crystallinity is expected to be relatively minor [107].
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
516 Applied Composite Materials (2025) 32:493–523
∆Hm
xc = ∗
× 100% (3)
∆Hm
Thermogravimetric Analysis (TGA) tests, are used to analyze the thermal weight loss of
the PA12-CF samples. During the testing, the samples are placed in ceramic crucibles and
heated from room temperature to 600 °C at a rate of 10 °C/min. Before to testing, nitrogen
gas is flowed at a rate of 100 ml/min to protect equipment, improve test accuracy, and
prevent sample oxidation. Figure 23 illustrates the PA12-CF TGA curves before and after
annealing. The results indicate that the initial temperatures of thermal degradation before
and after annealing are approximately 422 °C and 413 °C, respectively. The completion
temperatures of degradation are separately around 505 °C and 508 °C, with residual mass
percentages after degradation approximately 22.2% and 21.2%, respectively.
In summary, annealing significantly impacts the bending strength, the bending elastic
modulus, and fracture deflection of PA12 materials reinforced with 10 wt% short carbon
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 517
4 Conclusion
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
518 Applied Composite Materials (2025) 32:493–523
From the results presented above, it is seen that printing parameters of HFDM systems
have a direct impact on the resulting mechanical properties of printed composites. This
offers wide range of tunability on the material properties of extruded beads from FDM 3D
printing, which enables the manufacturing of customized functional graded structures (i.e.,
intricate parts with locally different mechanical responses).
Supplementary Information The online version contains supplementary material available at https://doi.
org/10.1007/s10443-024-10279-0.
Acknowledgements This work was supported by the National Natural Science Foundation of China (Grant
No. 52101381), the China Postdoctoral Science Foundation (Grant No. 2023M730455), the Department of
Education of Liaoning Province (Grant No. LJKMZ20220366), and the Fundamental Research Funds for the
Central Universities, Dalian Maritime University (Grant No. 3132024115).
Author Contributions Z.W. conceptualized the study, developed the methodology, and supervised the proj-
ect, including acquiring funding. Z.W. and B.Z. wrote the original draft. Z.W., B.Z., J.S., and J.W. conducted
experiments, performed formal analysis, managed data, conducted investigations, and contributed to the
visual presentation. All authors reviewed and edited the manuscript.
Data Availability No datasets were generated or analysed during the current study.
Declarations
References
1. Nieto, D.M., López, V.C., Molina, S.I.: Large-format polymeric pellet-based additive manufacturing for
the naval industry. Additive Manuf. 23, 79–85 (2018)
2. Goh, G.D., Wong, K.K., Tan, N., Seet, H.L., Nai, M.L.S.: Large-format additive manufacturing of poly-
mers: A review of fabrication processes, materials, and design. Virtual Phys. Prototyp. 19(1), e2336160
(2024)
3. Duty, C.E., Kunc, V., Compton, B., Post, B., Erdman, D., Smith, R., et al.: Structure and mechanical
behavior of Big Area Additive Manufacturing (BAAM) materials. Rapid Prototyp. J. 23(1), 181–189
(2017)
4. Ajinjeru, C., Kishore, V., Liu, P., Lindahl, J., Hassen, A.A., Kunc, V., et al.: Determination of melt
processing conditions for high performance amorphous thermoplastics for large format additive manu-
facturing. Additive Manuf. 21, 125–132 (2018)
5. Romani, A., Perusin, L., Ciurnelli, M., Levi, M.: Characterization of PLA feedstock after multiple recy-
cling processes for large-format material extrusion additive manufacturing. Mater. Today Sustain. 25,
100636 (2024)
6. Saavedra-Rojas, F.A., Bhandari, S., Lopez-Anido, R.A.: Environmental durability of Bio-based and
Synthetic Thermoplastic composites in large-format Additive Manufacturing. Polymers. 16(6), 787
(2024)
7. Nieto, D.M., Pintos, P.B., Sánchez, D.M., Rubio, S.I.M. (eds.): Large Format Additive Manufacturing
in Furniture Design with Novel Cork Based Polymeric Materials. International conference on The Digi-
tal Transformation in the Graphic Engineering; : Springer. (2022)
8. Love, L.J.: Utility of big area Additive Manufacturing (BAAM) for the Rapid Manufacture of Custom-
ized Electric Vehicles. Oak Ridge National Lab.(ORNL), ; (2015). Oak Ridge, TN (United States)
9. Vicente, C.M., Sardinha, M., Reis, L., Ribeiro, A., Leite, M.: Large-format additive manufacturing of
polymer extrusion-based deposition systems: Review and applications. Progress Additive Manuf. 8(6),
1257–1280 (2023)
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 519
10. Oskolkov, A.A., Trushnikov, D.N., Bezukladnikov, I.I.: Application of induction heating in the FDM/
FFF 3D manufacturing. J. Phys: Conf. Ser. 1730(1), 012005 (2021)
11. Krishnanand, S.V., Mittal, V., Branwal, A.K., Taufik, M. (eds.): Extruder Design in Pellets Operated 3D
Printers: A Review. Proceedings of the International Conference on Industrial and Manufacturing Sys-
tems (CIMS-2020) Optimization in Industrial and Manufacturing Systems and Applications; : Springer.
(2022)
12. Khan, A., Rahman, K., Kim, D.S., Choi, K.H.: Direct printing of copper conductive micro-tracks by
multi-nozzle electrohydrodynamic inkjet printing process. J. Mater. Process. Technol. 212(3), 700–706
(2012)
13. Ermolai, V., Irimia, A.I.: Influence of nozzle parameters in 3D printing under the manufacturing time.
Bull. Polytechnic Inst. Iași Mach. Constructions Sect. 67(3), 63–72 (2021)
14. Tezel, T., Kovan, V.: Determination of optimum production parameters for 3D printers based on nozzle
diameter. Rapid Prototyp. J. 28(1), 185–194 (2022)
15. Almuflih, A.S., Abas, M., Khan, I., Noor, S.: Parametric Optimization of FDM process for PA12-CF
parts using Integrated Response Surface Methodology, Grey Relational Analysis, and Grey Wolf Opti-
mization. Polymers. 16(11), 1508 (2024)
16. Zhang, X., Fan, W., Liu, T.: Fused deposition modeling 3D printing of polyamide-based composites and
its applications. Compos. Commun. 21, 100413 (2020)
17. Pejkowski, Ł., Seyda, J., Nowicki, K., Mrozik, D.: Mechanical performance of non-reinforced, carbon
fiber reinforced and glass bubbles reinforced 3D printed PA12 polyamide. Polym. Test. 118, 107891
(2023)
18. Walter, R., Selzer, R., Gurka, M., Friedrich, K.: Effect of filament quality, structure, and processing
parameters on the properties of fused filament fabricated short fiber-reinforced thermoplastics. In:
Friedrich, K., Walter, R., Soutis, C., Advani, S.G., Fiedler, I.H.B. (eds.) Structure and Properties of
Additive Manufactured Polymer Components, pp. 253–302. Woodhead Publishing (2020)
19. Andrew, J.J., Uddin, M.A., Kumar, S., Schiffer, A.: Mechanical and piezoresistive performance of addi-
tively manufactured carbon fiber/PA12 hybrid honeycombs. Thin-Walled Struct. 201, 111950 (2024)
20. Abderrafai, Y., Mahdavi, M.H., Sosa-Rey, F., Hérard, C., Navas, I.O., Piccirelli, N., et al.: Additive
manufacturing of short carbon fiber-reinforced polyamide composites by fused filament fabrication:
Formulation, manufacturing and characterization. Mater. Design. 214, 110358 (2022)
21. Zhuang, Y., Zou, B., Ding, S., Wang, X., Liu, J., Li, L.: Preparation of pre-impregnated continuous car-
bon fiber reinforced nylon6 filaments and the mechanical properties of 3D printed composites. Mater.
Today Commun. 35, 106163 (2023)
22. Yan, C., Hao, L., Xu, L., Shi, Y.: Preparation, characterisation and processing of carbon fibre/polyam-
ide-12 composites for selective laser sintering. Compos. Sci. Technol. 71(16), 1834–1841 (2011)
23. Liu, Y., Zhu, L., Zhou, L., Li, Y.: Microstructure and mechanical properties of reinforced polyamide 12
composites prepared by laser additive manufacturing. Rapid Prototyp. J. 25(6), 1127–1134 (2019)
24. Nar, K., Majewski, C., Lewis, R.: Evaluating the effect of solid lubricant inclusion on the friction and
wear properties of laser sintered Polyamide-12 components. Wear. 522, 204873 (2023)
25. Kausar, A.: Advances in carbon fiber reinforced polyamide-based composite materials. Adv. Mater. Sci.
19(4), 67–82 (2019)
26. Grieder, S., Zhilyaev, I., Küng, M., Brauner, C., Akermann, M., Bosshard, J., et al.: Consolidation of
additive manufactured continuous carbon fiber reinforced polyamide 12 composites and the develop-
ment of process-related numerical simulation methods. Polymers. 14(16), 3429 (2022)
27. Popescu, D., Zapciu, A., Amza, C., Baciu, F., Marinescu, R.: FDM process parameters influence over
the mechanical properties of polymer specimens: A review. Polym. Test. 69, 157–166 (2018)
28. Chacón, J.M., Caminero, M.A., García-Plaza, E., Núnez, P.J.: Additive manufacturing of PLA struc-
tures using fused deposition modelling: Effect of process parameters on mechanical properties and their
optimal selection. Mater. Design. 124, 143–157 (2017)
29. Raut, S., Jatti, V.S., Khedkar, N.K., Singh, T.: Investigation of the effect of built orientation on mechani-
cal properties and total cost of FDM parts. Procedia Mater. Sci. 6, 1625–1630 (2014)
30. Rayegani, F., Onwubolu, G.C.: Fused deposition modelling (FDM) process parameter prediction and
optimization using group method for data handling (GMDH) and differential evolution (DE). Int. J.
Adv. Manuf. Technol. 73, 509–519 (2014)
31. Sood, A.K., Ohdar, R.K., Mahapatra, S.S.: Parametric appraisal of mechanical property of fused deposi-
tion modelling processed parts. Mater. Design. 31(1), 287–295 (2010)
32. Mohamed, O.A., Masood, S.H., Bhowmik, J.L.: Mathematical modeling and FDM process parameters
optimization using response surface methodology based on Q-optimal design. Appl. Math. Model.
40(23–24), 10052–10073 (2016)
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
520 Applied Composite Materials (2025) 32:493–523
33. Mahapatra, S., Sood, A., Patel, S., Sahu, S.: Optimization of Process Parameters in Fused Deposi-
tion Modeling Using Weighted Principal Component Analysis. Administrative Staff College of India
(ASCI), Hyderabad, India (2009)
34. Durgun, I., Ertan, R.: Experimental investigation of FDM process for improvement of mechanical prop-
erties and production cost. Rapid Prototyp. J. 20(3), 228–235 (2014)
35. Liu, X., Zhang, M., Li, S., Si, L., Peng, J., Hu, Y.: Mechanical property parametric appraisal of fused
deposition modeling parts based on the gray Taguchi method. Int. J. Adv. Manuf. Technol. 89, 2387–
2397 (2017)
36. Fischer, D., Eßbach, C., Schönherr, R., Dietrich, D., Nickel, D.: Improving inner structure and proper-
ties of additive manufactured amorphous plastic parts: The effects of extrusion nozzle diameter and
layer height. Additive Manuf. 51, 102596 (2022)
37. Larsson, J., Lindström, P., Korin, C., Ekengren, J., Karlsson, P. (eds.): The influence of nozzle size on
the printing process and the mechanical properties of FFF-printed parts. International Conference on
Additive Manufacturing in Products and Applications; : Springer. (2023)
38. Czyżewski, P., Marciniak, D., Nowinka, B., Borowiak, M., Bieliński, M.: Influence of extruder’s nozzle
diameter on the improvement of functional properties of 3D-printed PLA products. Polymers. 14(2),
356 (2022)
39. Aliheidari, N., Christ, J., Tripuraneni, R., Nadimpalli, S., Ameli, A.: Interlayer adhesion and fracture
resistance of polymers printed through melt extrusion additive manufacturing process. Mater. Design.
156, 351–361 (2018)
40. Kuznetsov, V.E., Solonin, A.N., Urzhumtsev, O.D., Schilling, R., Tavitov, A.G.: Strength of PLA Com-
ponents Fabricated with fused Deposition Technology using a Desktop 3D printer as a function of geo-
metrical parameters of the process. Polymers. 10(3), 313 (2018)
41. Caminero, M., Chacón, J., García-Moreno, I., Rodríguez, G.: Impact damage resistance of 3D printed
continuous fibre reinforced thermoplastic composites using fused deposition modelling. Compos. Part.
B: Eng. 148, 93–103 (2018)
42. Fischer, S.: A material model for FE-simulation of UD composites. Appl. Compos. Mater. 23, 197–217
(2016)
43. Wang, Z., Smith, D.E.: A fully coupled simulation of planar deposition flow and fiber orientation in
polymer composites additive manufacturing. Materials. 14(10), 2596 (2021)
44. Advani, S.G., Tucker, C.L. III: The use of tensors to describe and predict fiber orientation in short fiber
composites. J. Rheol. 31(8), 751–784 (1987)
45. Song, Y., Gandhi, U., Pérez, C., Osswald, T., Vallury, S., Yang, A.: Method to account for the fiber ori-
entation of the initial charge on the fiber orientation of finished part in compression molding simulation.
Compos. Part A: Appl. Sci. Manufac. 100, 244–254 (2017)
46. Colón Quintana, J.L., Slattery, L., Pinkham, J., Keaton, J., Lopez-Anido, R.A., Sharp, K.: Effects of
fiber orientation on the coefficient of thermal expansion of fiber-filled polymer systems in large format
polymer extrusion-based additive manufacturing. Materials. 15(8), 2764 (2022)
47. Pibulchinda, P., Barocio, E., Pipes, R.B.: Influence of fiber orientation on deformation of additive manu-
factured composites. Additive Manuf. 49, 102483 (2022)
48. Zhuang, Y., Zou, B., Ding, S., Wang, P.: Shear and Tensile behaviors of Fiber-Reinforced Resin Matrix
composites printed by the FDM Technology. Coatings. 12(7), 1000 (2022)
49. Huang, H., Gao, X., Teng, L.: Fiber alignment and its effect on mechanical properties of UHPC: An
overview. Constr. Build. Mater. 296, 123741 (2021)
50. Parmiggiani, A., Prato, M., Pizzorni, M.: Effect of the fiber orientation on the tensile and flexural behav-
ior of continuous carbon fiber composites made via fused filament fabrication. Int. J. Adv. Manuf.
Technol. 114, 2085–2101 (2021)
51. Devireddy, S.B.R., Biswas, S.: Effect of Fiber geometry and representative volume element on Elastic
and Thermal properties of Unidirectional Fiber-Reinforced composites. J. Compos. 2014(1), 629175
(2014)
52. Love, L.J., Kunc, V., Rios, O., Duty, C.E., Elliott, A.M., Post, B.K., et al.: The importance of carbon
fiber to polymer additive manufacturing. J. Mater. Res. 29(17), 1893–1898 (2014)
53. Ning, F., Cong, W., Qiu, J., Wei, J., Wang, S.: Additive manufacturing of carbon fiber reinforced ther-
moplastic composites using fused deposition modeling. Compos. Part. B: Eng. 80, 369–378 (2015)
54. Fu, S.-Y., Lauke, B.: Effects of fiber length and fiber orientation distributions on the tensile strength of
short-fiber-reinforced polymers. Compos. Sci. Technol. 56(10), 1179–1190 (1996)
55. Banakar, P., Shivananda, H., Niranjan, H.: Influence of fiber orientation and thickness on tensile proper-
ties of laminated polymer composites. Int. J. Pure Appl. Sci. Technol. 9(1), 61 (2012)
56. Wang, Z., Zhou, Y., Mallick, P.: Effects of temperature and strain rate on the tensile behavior of short
fiber reinforced polyamide-6. Polym. Compos. 23(5), 858–871 (2002)
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 521
57. Mortazavian, S., Fatemi, A.: Effects of fiber orientation and anisotropy on tensile strength and elastic
modulus of short fiber reinforced polymer composites. Compos. part. B: Eng. 72, 116–129 (2015)
58. Kim, J.-W., Lee, D.-G.: Effect of fiber orientation and fiber contents on the tensile strength in fiber-
reinforced composites. J. Nanosci. Nanotechnol. 10(5), 3650–3653 (2010)
59. Spoerk, M., Savandaiah, C., Arbeiter, F., Traxler, G., Cardon, L., Holzer, C., et al.: Anisotropic prop-
erties of oriented short carbon fibre filled polypropylene parts fabricated by extrusion-based additive
manufacturing. Compos. Part A: Appl. Sci. Manufac. 113, 95–104 (2018)
60. Ferreira, R.T.L., Amatte, I.C., Dutra, T.A., Bürger, D.: Experimental characterization and micrography
of 3D printed PLA and PLA reinforced with short carbon fibers. Compos. Part. B: Eng. 124, 88–100
(2017)
61. Nergün, M., Önel, N., Vatandaş, B.B., Uşun, A., Gümrük, R.: Obtaining High Mechanical Properties
Polyamide-continuous Carbon Fiber Reinforced Thermoplastic composites with Infrared Heating.
Avrupa Bilim ve Teknoloji Dergisi. 36, 222–226 (2022)
62. Vatandaş, B.B., Uşun, A., Gümrük, R.: Mechanical performances of continuous carbon fiber reinforced
PEEK (polyether ether ketone) composites printed in a vacuum environment. J. Manuf. Process. 120,
579–594 (2024)
63. D’Amico, T., Peterson, A.M.: Bead parameterization of desktop and room-scale material extrusion
additive manufacturing: How print speed and thermal properties affect heat transfer. Additive Manuf.
34, 101239 (2020)
64. Zhang, W., Cotton, C., Sun, J., Heider, D., Gu, B., Sun, B., et al.: Interfacial bonding strength of short
carbon fiber/acrylonitrile-butadiene-styrene composites fabricated by fused deposition modeling. Com-
pos. Part. B: Eng. 137, 51–59 (2018)
65. Masood, S.H., Mau, K., Song, W. (eds.): Tensile Properties of Processed FDM Polycarbonate Material.
Materials Science Forum. Trans Tech Publ (2010)
66. Kundurthi, S., Tran, F., Chen, S., Mapkar, J., Haq, M.: Bead geometry–induced stress concentration fac-
tors in material extrusion polymer additive manufacturing. Rapid Prototyp. J. 29(7), 1438–1452 (2023)
67. Wang, Z., Wang, J., Zhang, Y., Li, Y., Li, Y.: Exploring the effects of Processing parameters on the Flex-
ural performance of polylactic acid fabricated through a customized high extrusion rate fused filament
fabrication system. J. Mater. Eng. Perform. (2023). https://doi.org/10.1007/s11665-023-09003-z
68. Rimašauskas, M., Jasiūnienė, E., Kuncius, T., Rimašauskienė, R., Cicėnas, V.: Investigation of influ-
ence of printing parameters on the quality of 3D printed composite structures. Compos. Struct. 281,
115061 (2022)
69. Patel, R., Desai, C., Kushwah, S., Mangrola, M.: A review article on FDM process parameters in 3D
printing for composite materials. Mater. Today: Proc. 60, 2162–2166 (2022)
70. Korkees, F., Allenby, J., Dorrington, P.: 3D printing of composites: Design parameters and flexural
performance. Rapid Prototyp. J. 26(4), 699–706 (2020)
71. Triyono, J., Sukanto, H., Saputra, R.M., Smaradhana, D.F.: The effect of nozzle hole diameter of 3D
printing on porosity and tensile strength parts using polylactic acid material. Open. Eng. 10(1), 762–768
(2020)
72. Chacón, J.M., Caminero, M., Núñez, P.J., García-Plaza, E., Bécar, J.P.: Effect of nozzle diameter on
mechanical and geometric performance of 3D printed carbon fibre-reinforced composites manufactured
by fused filament fabrication. Rapid Prototyp. J. 27(4), 769–784 (2021)
73. Standard, A.: Standard test methods for flexural properties of unreinforced and reinforced plastics and
electrical insulating materials. ASTM D790. Annual book of ASTM standards. (1997)
74. Basgul, C., Yu, T., MacDonald, D.W., Siskey, R., Marcolongo, M., Kurtz, S.M.: Does annealing improve
the interlayer adhesion and structural integrity of FFF 3D printed PEEK lumbar spinal cages? J. Mech.
Behav. Biomed. Mater. 102, 103455 (2020)
75. Singh, S., Singh, M., Prakash, C., Gupta, M.K., Mia, M., Singh, R.: Optimization and reliability analy-
sis to improve surface quality and mechanical characteristics of heat-treated fused filament fabricated
parts. Int. J. Adv. Manuf. Technol. 102, 1521–1536 (2019)
76. Rabbi, M.F., Chalivendra, V.: Improvement in interfacial fracture toughness of multi-material additively
manufactured composites through thermal annealing. Forces Mech. 5, 100051 (2021)
77. Su, R., Zhang, Z., Love, B.J., Shih, A.J.: Fused filament fabrication of Nylon beyond the glass transition
temperature in a thermally-insulated machine. Manuf. Lett. 35, 797–804 (2023)
78. Butt, J., Bhaskar, R.: Investigating the effects of annealing on the mechanical properties of FFF-printed
thermoplastics. J. Manuf. Mater. Process. 4(2), 38 (2020)
79. Braconnier, D.J., Dunn, R.M., Wetzel, E.D., Erb, R.M.: The role of crystallization and annealing on the
thermal conductivity of material extrusion additively manufactured parts. Additive Manuf. 89, 104265
(2024)
80. Rajpurohit, S.R., Dave, H.K.: Flexural strength of fused filament fabricated (FFF) PLA parts on an
open-source 3D printer. Adv. Manuf. 6, 430–441 (2018)
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
522 Applied Composite Materials (2025) 32:493–523
81. Dev, S., Srivastava, R.: Optimization of fused deposition modeling (FDM) process parameters for flex-
ural strength. Mater. Today: Proc. 44, 3012–3016 (2021)
82. Leon, R., Ling, T., Lease, J.: Optimizing layer thickness and print orientation of 3D objects for enhanced
mechanical property using Structo 3D printers. https://docplayer.net/39789245-Optimizing-layer-thick-
ness-and-print-orientation-of-3d-objects-forenhanced-mechanical-property-using-structo-3d-printers.
html (2017)
83. Mohamed, O.A., Masood, S.H., Bhowmik, J.L.: Optimization of fused deposition modeling process
parameters: A review of current research and future prospects. Adv. Manuf. 3, 42–53 (2015)
84. Abdullah, Z., Ting, H., Ali, M., Fauadi, M., Kasim, M., Hambali, A., et al.: The effect of layer thickness
and raster angles on tensile strength and flexural strength for fused deposition modeling (FDM) parts. J.
Adv. Manuf. Technol. (JAMT). 12(1), 147–158 (2018)
85. Stamopoulos, A.G., Ilaria Scipioni, S., Lambiase, F.: Experimental characterization of the interlayer
fracture toughness of FDM components. Compos. Struct. 320, 117213 (2023)
86. Butt, J., Bhaskar, R., Mohaghegh, V.: Investigating the influence of material extrusion rates and line
widths on FFF-Printed graphene-enhanced PLA. J. Manuf. Mater. Process. 6(3), 57 (2022)
87. Ding, S., Zou, B., Zhang, P., Liu, Q., Zhuang, Y., Feng, Z., et al.: Layer thickness and path width setting
in 3D printing of pre-impregnated continuous carbon, glass fibers and their hybrid composites. Additive
Manuf. 83, 104054 (2024)
88. Valvez, S., Reis, P.N., Ferreira, J.A.: Effect of annealing treatment on mechanical properties of
3D-Printed composites. J. Mater. Res. Technol. 23, 2101–2115 (2023)
89. Coogan, T.J., Kazmer, D.O.: Modeling of interlayer contact and contact pressure during fused filament
fabrication. J. Rheol. 63(4), 655–672 (2019)
90. Ding, S., Zou, B., Zhuang, Y., Wang, X., Li, L., Liu, J.: Hybrid layout and additive manufacturing of
continuous carbon/glass fibers reinforced composites, and its effect on mechanical properties. Compos.
Struct. 319, 117133 (2023)
91. König, M., Diekmann, J., Lahres, M., Middendorf, P.: Experimental investigation of process-structure
effects on interfacial bonding strength of a short carbon fiber/polyamide composite fabricated by fused
filament fabrication. Progress Additive Manuf. 7:593–607. https://doi.org/10.1007/s40964-021-00249-
4 (2022)
92. Ferreira, I., Melo, C., Neto, R., Machado, M., Alves, J.L., Mould, S.: Study of the annealing influence
on the mechanical performance of PA12 and PA12 fibre reinforced FFF printed specimens. Rapid Pro-
totyp. J. 26(10), 1761–1770 (2020)
93. Zhang, L., Wu, C. (eds.): Preparation method for metallographic specimen of Iron-Carbon and silicon-
aluminium alloy. Journal of Physics: Conference Series; : IOP Publishing. (2022)
94. Yan, J., Demirci, E., Ganesan, A., Gleadall, A.: Extrusion width critically affects fibre orientation in
short fibre reinforced material extrusion additive manufacturing. Additive Manuf. 49, 102496 (2022)
95. Yan, J., Demirci, E., Gleadall, A.: 3D short fibre orientation for universal structures and geometries in
material extrusion additive manufacturing. Additive Manuf. 69, 103535 (2023)
96. Kartal, F., Kaptan, A.: Effects of annealing temperature and duration on mechanical properties of PLA
plastics produced by 3D Printing. Eur. Mech. Sci. 7(3), 152–159 (2023)
97. Stojković, J.R., Turudija, R., Vitković, N., Górski, F., Păcurar, A., Pleşa, A., et al.: An experimental
study on the impact of layer height and annealing parameters on the tensile strength and dimensional
accuracy of FDM 3D printed parts. Materials. 16(13), 4574 (2023)
98. Bhandari, S., Lopez-Anido, R.A., Gardner, D.J.: Enhancing the interlayer tensile strength of 3D printed
short carbon fiber reinforced PETG and PLA composites via annealing. Additive Manuf. 30, 100922
(2019)
99. Papon, E.A., Haque, A., Spear, S.K.: Effects of functionalization and annealing in enhancing the interfa-
cial bonding and mechanical properties of 3D printed fiber-reinforced composites. Mater. Today Com-
mun. 25, 101365 (2020)
100. Valvez, S., Silva, A., Reis, P., Berto, F.: Annealing effect on mechanical properties of 3D printed com-
posites. Procedia Struct. Integr. 37, 738–745 (2022)
101. Desio, G.P., Rebenfeld, L.: Crystallization of fiber-reinforced poly (phenylene sulfide) composites. I.
Experimental studies of crystallization rates and morphology. J. Appl. Polym. Sci. 44(11), 1989–2001
(1992)
102. Desio, G.P., Rebenfeld, L.: Crystallization of fiber-reinforced poly (phenylene sulfide) composites. II.
Modeling the crystallization kinetics. J. Appl. Polym. Sci. 45(11), 2005–2020 (1992)
103. Ruan, C., Ouyang, J., Liu, S.: Multi-scale modeling and simulation of crystallization during cooling in
short fiber reinforced composites. Int. J. Heat Mass Transf. 55(7–8), 1911–1921 (2012)
104. Bahrami, M., Abenojar, J., Martínez, M.A.: Comparative characterization of hot-pressed polyamide 11
and 12: Mechanical, thermal and durability properties. Polymers. 13(20), 3553 (2021)
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Applied Composite Materials (2025) 32:493–523 523
105. Kaiser, G., Füglein, E., Jeschke, Y., Kapsch, E., Steidl, D.: Handbook Differential Scanning Calorimetry
(DSC) on Polymers. NETZSCH-Gerätebau GmbH (2015)
106. Quintanilla, L., Alonso, M., Rodríguez-Cabello, J., Pastor, J.: Structural analysis of poly (ethylene tere-
phthalate) reinforced with glass fiber: Thermal behavior and correlation between PA‐FTIR and DSC
measurements. J. Appl. Polym. Sci. 59(5), 769–774 (1996)
107. Lee, T., Boey, F., Khor, K.: On the determination of polymer crystallinity for a thermoplastic PPS com-
posite by thermal analysis. Compos. Sci. Technol. 53(3), 259–274 (1995)
Publisher’s Note Springer Nature remains neutral with regard to jurisdictional claims in published maps and
institutional affiliations.
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a
publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manu-
script version of this article is solely governed by the terms of such publishing agreement and applicable law.
13
Content courtesy of Springer Nature, terms of use apply. Rights reserved.
Terms and Conditions
Springer Nature journal content, brought to you courtesy of Springer Nature Customer Service Center
GmbH (“Springer Nature”).
Springer Nature supports a reasonable amount of sharing of research papers by authors, subscribers
and authorised users (“Users”), for small-scale personal, non-commercial use provided that all
copyright, trade and service marks and other proprietary notices are maintained. By accessing,
sharing, receiving or otherwise using the Springer Nature journal content you agree to these terms of
use (“Terms”). For these purposes, Springer Nature considers academic use (by researchers and
students) to be non-commercial.
These Terms are supplementary and will apply in addition to any applicable website terms and
conditions, a relevant site licence or a personal subscription. These Terms will prevail over any
conflict or ambiguity with regards to the relevant terms, a site licence or a personal subscription (to
the extent of the conflict or ambiguity only). For Creative Commons-licensed articles, the terms of
the Creative Commons license used will apply.
We collect and use personal data to provide access to the Springer Nature journal content. We may
also use these personal data internally within ResearchGate and Springer Nature and as agreed share
it, in an anonymised way, for purposes of tracking, analysis and reporting. We will not otherwise
disclose your personal data outside the ResearchGate or the Springer Nature group of companies
unless we have your permission as detailed in the Privacy Policy.
While Users may use the Springer Nature journal content for small scale, personal non-commercial
use, it is important to note that Users may not:
1. use such content for the purpose of providing other users with access on a regular or large scale
basis or as a means to circumvent access control;
2. use such content where to do so would be considered a criminal or statutory offence in any
jurisdiction, or gives rise to civil liability, or is otherwise unlawful;
3. falsely or misleadingly imply or suggest endorsement, approval , sponsorship, or association
unless explicitly agreed to by Springer Nature in writing;
4. use bots or other automated methods to access the content or redirect messages
5. override any security feature or exclusionary protocol; or
6. share the content in order to create substitute for Springer Nature products or services or a
systematic database of Springer Nature journal content.
In line with the restriction against commercial use, Springer Nature does not permit the creation of a
product or service that creates revenue, royalties, rent or income from our content or its inclusion as
part of a paid for service or for other commercial gain. Springer Nature journal content cannot be
used for inter-library loans and librarians may not upload Springer Nature journal content on a large
scale into their, or any other, institutional repository.
These terms of use are reviewed regularly and may be amended at any time. Springer Nature is not
obligated to publish any information or content on this website and may remove it or features or
functionality at our sole discretion, at any time with or without notice. Springer Nature may revoke
this licence to you at any time and remove access to any copies of the Springer Nature journal content
which have been saved.
To the fullest extent permitted by law, Springer Nature makes no warranties, representations or
guarantees to Users, either express or implied with respect to the Springer nature journal content and
all parties disclaim and waive any implied warranties or warranties imposed by law, including
merchantability or fitness for any particular purpose.
Please note that these rights do not automatically extend to content, data or other material published
by Springer Nature that may be licensed from third parties.
If you would like to use or distribute our Springer Nature journal content to a wider audience or on a
regular basis or in any other manner not expressly permitted by these Terms, please contact Springer
Nature at