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Suitability of PLATCP For Fused Deposition
Suitability of PLATCP For Fused Deposition
Sung-Hoon Ahn, Michael Montero, Dan Odell, Shad Roundy, Paul K. Wright, (2002),"Anisotropic material properties of fused
deposition modeling ABS", Rapid Prototyping Journal, Vol. 8 Iss 4 pp. 248-257 http://dx.doi.org/10.1108/13552540210441166
Brian N. Turner, Robert Strong, Scott A. Gold, (2014),"A review of melt extrusion additive manufacturing processes: I. Process
design and modeling", Rapid Prototyping Journal, Vol. 20 Iss 3 pp. 192-204 http://dx.doi.org/10.1108/RPJ-01-2013-0012
Q. Sun, G.M. Rizvi, C.T. Bellehumeur, P. Gu, (2008),"Effect of processing conditions on the bonding quality of FDM polymer
filaments", Rapid Prototyping Journal, Vol. 14 Iss 2 pp. 72-80 http://dx.doi.org/10.1108/13552540810862028
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Abstract
Purpose – Fused deposition modeling (FDM) is a layer by layer technology with the potential to create complex and individual parts from
thermoplastic materials such as ABS. The use of Polylactic acid (PLA) and tricalcium phosphate (TCP) as resorbable composite is state of the art in tissue
engineering and maxillofacial surgery. The purpose of this paper is to evaluate the processing conditions and the performance of parts (e.g. mechanical
properties) manufactured with a FDM machine.
Design/methodology/approach – In this paper, the general suitability of PLA for the processing with FDM is evaluated and material specific effects
(e.g. crystallization and shrinkage) are shown. Therefore, the characterization of the semi-crystalline biodegradable material by thermal, mechanical
and microscopic analysis is carried out.
Findings – Facts, which affect the functional properties of the samples, are analyzed. Among them, the processing temperature and sample size
significantly affect the morphology of the final components. Components from PLA/TCP with sufficient mechanical properties for their potential use as
scaffolds are obtained.
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Originality/value – Thus, the paper shows that by thermal analysis it is possible to identify major influences on processing and part properties.
Keywords Advanced manufacturing technologies, Modelling, Mechanical properties of materials, Composite materials, Fused deposition modelling
500
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
Table I Biomaterials investigated in FDM Thermal analysis of PLA was done by means of differential
scanning calorimetry (DSC Q1000, TA Instruments) to
Material Reference
investigate the change in thermal history. In first instance, the
PCL Hutmacher et al. (2000), materials were dried according to the manufacturers
Zein et al. (2002), Chim et al. (2006) requirements. Once the sufficient drying was carried out,
HA Bose et al. (1999) PLA was compound with 2.5 and 5.0 wt.% b-TCP at 808C
PP-b-TCP Kalita et al. (2003) during one hour in a MP-M mixer (Somakon GmbH). Then
POT/PBT Moroni et al. (2006) the material was extruded in a micro extruder (ED-N20-25D,
PCL-b-TCP Chim et al. (2006) Extrudex Kunststoffmaschinen GmbH) to filaments with a
b-TCP Bose et al. (2003) diameter of 1.65 ^ 0.05 mm. For the cooling and calibration
of the filament the extruder counts with a cool and calibration
bath, and a belt-haul off.
(3D-Bioplottere, EnvisionTEC) available for drug release The obtained filaments were processed in a Stratasys FDM
and tissue engineering applications (Wendel et al., 2008). 8000 machine. As the filaments with a b-TCP content of 5.0
Among the shown biomaterials suitable for being modeled by wt.% were to brittle for the processing in the FDM machine
fused deposition, poly(L-lactic acid) (PLLA)/TCP composite the investigation were only carried out with a filler content of
scaffolds seem to have best mechanical properties (Xiong et al., 2.5 wt.%. In order to investigate the influence of processing
2001, 2002; Yan et al., 2003). temperature on the mechanical performance of FDM-parts,
To know about the material behavior during processing and 1:2 samples for short-term tensile tests according to DIN EN
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the resulting part properties, the characterization of new ISO 527-1,-2 were processed at three different temperatures
materials by thermal and microscopic analysis is crucial. (215, 225 and 2358C) and a chamber temperature of 408C.
These tests will be carried out in this paper in order to
With the aim of analyzing the influence of the part size built
evaluate the processing conditions and the performance of
with FDM, a set of five full sized (1:1) specimens was built at
parts (e.g. mechanical properties) manufactured with a FDM
2358C. Thus, in this single investigation it is possible to
machine.
analyze the influence of a variation in time between the single
paths that are molten on the resulting morphology. As the
2. Materials and methods sample built with the highest nozzle temperature (2358C) may
lead to the highest recrystallization of the subjacent layer only
For this investigation, Polylactide Biomerw L9000, supplied
this temperature was chosen.
by the company Biomer, Germany and b-TCP (nanoXIM
Other influencing variables on the component properties are
TCP202), provided by Fluidinova, Portugal are the selected
content, geometry and dispersion of the filler within the
materials.
Commercially available polylactic acid (PLA) are in general polymeric matrix as they can affect the bonding and
copolymers of PLLA and poly(D,L-lactic acid) (PDLLA), solidification process. With pvT-measurements, using a pvT
which are produced from L-lactides and D,L-lactides, 100 (SWO Polymertechnik GmbH), an estimation of the change
respectively. PLA polymers with a L-lactide content more in volume of the later component during the solidification was
than cL , 90% tend to be crystalline while a lower amount done and the influence of the filler was investigated.
results in amorphous PDLLA (Lim et al., 2008). Thermogravimetric analysis was done using a TGA High
TCP Ca3(PO4)2 is one of the main elements of bone and Resolution 2950 (TA Instruments) and microscopic structure
thus an ideal implant material, which degrades in replacing studies (bright and polarized field illuminated microscopic
natural tissues. It enables the regeneration of tissue, as it is micrographs) were performed to assess the distribution of TCP,
an osteoconductive material (Cao and Hench, 1996). and to analyze the crystallization effects and resulting
The selected b-TCP is gained by a spray drying process and morphology. Additionally, SEM images were used to
has an average particle size of 5 ^ 1 mm to be easily dispersed investigate layer bonding and the fracture mirror of
in the polymer matrix. components after tensile testing.
501
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
measuring the heat of fusion and heat of recrystallization from consistent with those obtained from DSC-measurements.
DSC, with (Ehrenstein et al., 2003): PLA without filler behaves like an amorphous material, but
DH total ¼ DH melt 2 DH recrystallization once the material is extruded, modeled and has TCP within
the matrix, the behavior of the polymer is semi-crystalline.
DH total Figure 3 shows only one change of slope in the curve, relating
K¼ · 100%
DH Om specific volume with temperature, due to the glass transition
temperature. On the other hand, Figure 4 shows two changes
in slope, the first is due to crystallization (T , 115-1258C),
Figure 1 Differential scanning calorimetry – heating
and the second is caused by the glass transition temperature
0.5 (T , 608C). Nevertheless, in both cases the specific volume
heating Biomer L9000 DSC - 1. Heating change between molten and solid state is comparable. Low
0.0 107.1°C contraction in volume is an advantage for FDM as the
97.5°C
167.9°C filaments are solidified layer-by-layer unlike SLS, where a
Heat Flow [W/g]
502
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
Table III Crystallinity degree of the material according to the process stage (integral value)
Heat of fusion Heat of recrystallization
Process stage DHmelt (J/g) DHrecrystallization (J/g) Crystallinity K (%)
Granules 44.7 0.0 48.1
Extrudate 35.1 30.7 4.8
FDM-part 39.4 21.5 19.3
Table IV Crystallinity degree in different heights of FDM tensile bars Figure 4 Specific volume change of PLA þ 2.5 wt.% TCP when cooling
with varying processing parameters
1.00
Position Hmelt Hrecrystallization Htotal Crystallinity K 1 bar Biomer L9000 + 2.5%TCP
(mm) (J/g) (J/g) (J/g) (%) 0.95 200 bar
400 bar
800 bar
0.90 1,200 bar
0.85
0.80
0.75
∆v1,0 bar = 0.1154 [cm3/g]
0.70
20 40 60 80 100 120 140 160 180 200 220
Temperature [°C]
503
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
support structures that have to be removed manually. Parts semi-crystalline. This sample has a small superior opaque
presented an appropriate E-modulus for a later medical use, amorphous region at the upper layers which was also proven by
as Figure 6 shows. According to Ruffieux (2004), the stiffness DSC measurements (Table IV). The formation of crystals is
of an implant should range between 2,000 and 5,000 N/mm2. reduced to the center of the bottom layers (bottom of the
For the current short term tensile test the outcome for sample) with decreasing temperatures. Therefore, there is a
stiffness was 2,691 N/mm2 at a FDM nozzle temperature of remarkable relation between the processing temperature and
2158C, 3,122 N/mm2 at 2258C, and 2,730 N/mm2 at 2358C. the morphology of the final FDM-part. In the image of the 1:1
In accordance with Figure 6, the processing temperature sample, the comprised crystalline and amorphous regions are
which results in best mechanical performance is 2258C. shown more in detail. By taking a more detailed look into
The specimens that present the highest standard deviation morphology and filler distribution it can be observed that TCP
are the ones built at the lowest temperature. The parts with is evenly distributed in the polymer matrix (Figure 8).
the lowest tensile strength and elongation at break were By means of scaling of the part size, the thermal processing
manufactured at 2358C. conditions are changed, too. Also in the 1:1 tensile bar semi-
The cooling rate of the material is related with the processing crystalline areas are formed at the center of the cross section but
temperature and affects the degree of crystallinity and the preferred at the interface between rods. Especially the outer
morphology in the thermoplastic which, simultaneously, affects areas of single rods are heated several times, when a new layer of
the mechanical properties of the specimen and its molten material is deposited and thus recrystallization can take
biodegradability. The amorphous regions present faster place. Due to those significant differences in the transmitted
degradation and resorption in vivo, and higher diffusion light images, microtome cuts were collected top down as well as
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coefficients, in comparison to the semi-crystalline structures, bottom up and the degree of crystallinity was determined using
which have slower resorption in vivo and better mechanical DSC measurements (Table IV). A change from 8.35 percent
properties during degradation (Anderson and Shive, 1997). (upper regions) up to 40.72 percent (bottom regions) was
The morphology of the FDM-parts is visible in the obtained which has a high influence on mechanical properties
transmitted light images with polarized light taken of and the degradation behavior.
microtome cuts from FDM tensile bars at different nozzle Pieces have also imperfections due to the way of their
temperatures (Figure 7). In the plan view, it is visible that big manufacturing, layer-by-layer. In the presented micrographs, it
pores can still remain in the cross section and the accuracy is is also possible to identify remaining gaps in each part. Those
still bad. This can potentially be avoided with different gaps affect the mechanical performance of the part and act as
pathways generated by the software and a closer view on the weak points under load. Consequently, there may be the start of
processing behavior of PLA. Nevertheless, it is possible to fractures when load is exerted. Thus, SEM images of the
analyze the differences in structure and morphology of the layer fracture mirror were taken to analyze the mechanisms of break.
wise generated parts. Semi-crystalline areas of the samples are The fracture surface is in general brittle and in some areas the
seen translucent due to the changed optical diffraction of the interfacial bonding of single layers is visible (Figure 9).
dense packed crystals and can be distinguished from
the predominantly amorphous and thus transparent areas. 3.5 Influence of part size
The wide bright region of the bar with a nozzle temperature Figure 6 shows that there is a direct dependence between the
of 2358C indicates that mostly of the cross section is part size and the mechanical properties of the specimen.
Figure 6 Influence of processing temperature and size of specimens in mechanical properties of parts
5,000 40 2.0
E-modulus
Stress at Break 35
Tensile sress at break σbreak [N/mm2]
Elongation at Break
Modulus of Elasticity E [N/mm2]
4,000
Elongation at Break εbreak [%]
30 1.5
25
3,000
20 1.0
2,000
15
10 0.5
1,000
5
0 0 0.0
)
)
:2
:2
:2
:1
(1
(1
(1
(1
C
C
5°
5°
5°
5°
21
22
23
23
=
=
T
504
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
Figure 7 Transmitted light (polarized) images taken of microtome cuts from FDM tensile bars
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Notes: PLA/TCP 1:2 215°C (top left); PLA/TCP 1:2 225°C (top right); PLA/TCP 1:2 235°C
(bottom left); PLA/TCP 1:1 235°C (bottom right)
Figure 8 Transmitted light (polarized) and bright field image taken of microtome cuts from a FDM tensile bar (PLA/TCP 1:2 2358C) in order to show TCP
distribution
Bigger parts exhibit higher stiffness. This is due to the amount temperature on the parts size and tolerances was observed
of rasters that draw the path during the construction of a layer. (Table VI). All samples have an increased cross-section
Big parts are manufactured with the same raster diameter as compared to the nominal size – this has to be adjusted by the
small parts, and therefore they need more rasters in order to scaling factors when a robust process is set-up.
build every single layer than the smaller specimens.
Additionally, the influence of weak points on the surface is 4. Summary and outlook
diminished due to the higher cross section. The elastic modulus The main objective of this work was to process a biodegradable
of the 1:1 specimens is even higher than of the 1:2 specimens thermoplastic part by FDM and to understand the thermal
built at 2258C. Bigger specimens have a higher tensile strength effects that occur with this special polymer.
and elongation at break due to a better accuracy and density of Samples were manufactured at three different nozzle
the sample. On the other hand, the accuracy of the parts was temperatures in order to establish the influence of the
investigated but no significant influence of the processing processing temperature and to be evaluated with the short-
505
Suitability of PLA/TCP for fused deposition modeling Rapid Prototyping Journal
Dietmar Drummer, Sandra Cifuentes-Cuéllar and Dominik Rietzel Volume 18 · Number 6 · 2012 · 500 –507
Figure 9 SEM images of the fracture surface made from PLA/TCP 1:2 2358C
Table VI Nominal and real size of tensile bars processing parameters and the resulting morphology. Thus,
processing conditions influence the crystallinity of the implant
Width (mm) Thickness (mm) and this subsequently has severe effects on the degradation
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Nominal size 1:1 10.0 4.0 behavior and time. In knowing this behavior a special implant
Nominal size 1:2 5.0 2.0 design can help to generate selectively semi-crystalline or
amorphous areas to achieve long lasting mechanical properties
PLA/TCP 1:1 2358C 10.95 ^ 0.10 4.50 ^ 0.46
and a high degradation speed.
PLA/TCP 1:2 2358C 5.50 ^ 0.27 2.62 ^ 0.37
PLA/TCP 1:2 2258C 5.59 ^ 0.40 2.86 ^ 0.30
PLA/TCP 1:2 2158C 5.49 ^ 0.16 2.79 ^ 0.27 References
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No. 3, pp. 425-34 (Kidlington, ROYAUME-UNI: Dominik Rietzel can be contacted at: rietzel@lkt.
Elsevier). uni-erlangen.de
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