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(Download PDF) Four Dimensional Printing For Clinical Dentistry Rupinder Singh Ravinder Sharma Nishant Ranjan Full Chapter PDF
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Four-Dimensional Printing for Clinical Dentistry
Rupinder Singh, Ravinder Sharma, and Nishant Ranjan, Guru Nanak Dev Engineering College, Ludhiana, India
r 2017 Elsevier Inc. All rights reserved.
1 Introduction 1
2 Screw Extrusion 2
2.1 Types of Screw Extrusion Processes 2
2.2 TSE 2
3 FDM 4
3.1 Advantages of FDM Process 4
3.2 Disadvantages of FDM Process 4
4 Differential Scanning Calorimetry 5
5 Case Study 5
5.1 Materials Used 5
5.1.1 Biocompatible grade of PVC 5
5.1.2 Biocompatible grade of PP 6
5.1.3 HAp 6
5.2 Experimentation 6
5.3 Result and Discussions 9
5.3.1 Optimizing process parameters of TSE 9
5.3.1.1 Mechanical properties 9
5.3.1.1.1 Peak load 9
5.3.1.1.2 Break load 11
5.3.1.1.3 Young’s modulus 12
5.3.1.2 Material properties 12
5.3.1.3 Shore-D hardness 13
5.3.1.4 Dimensional analysis 16
5.3.1.5 Thermal properties 17
5.3.2 Parametric optimization of FDM 18
5.3.2.1 Surface roughness 18
5.3.2.2 Shore-D hardness 19
5.3.2.3 Dimensional analysis 21
5.3.2.4 Tensile testing 22
5.3.2.4.1 Peak load 23
5.3.2.4.2 Break load 26
5.3.2.5 Microscopic analysis 26
6 Conclusions 26
Acknowledgment 27
References 27
1 Introduction
The low cost and remarkable properties like strength, temperature/chemically resistant, nonconductivity, and reprocess or reusable
ability (Rosato et al., 2001) of polymers have attracted the interest of researchers for their use in various applications in the fields of
engineering, aerospace, biomedical science, etc. Thermoplastics materials having low melting point and could be easily molded
into variety of shapes by heating up (Bodner, 2004). The biocompatibility of some polymers makes them possible for use in
biomedical application. The polymers like polyvinyl chloride (PVC), polypropylene (PP), polyether ether ketone (PEEK), poly
lactic acid (PLA), etc. are the most widely used polymers in the biomedical field, particularly in the field of tissue engineering and
drug delivery.
Biocompatibility is defined as adaptability of some foreign component by the body environment without producing any
adverse effect to the functionality of the system. In medical science, biocompatibility is known as the interaction of any medical
part or component material with the tissue or living system. So in general a biocompatible object does not provide any harm to the
patient (Lendlein and Sisson, 2011; Tian et al., 2012). Most plastics intended for medical devices, including medical grades of PVC,
polyethylene, polycarbonate, PEEK, Ultem PEI, PP, poly-sulfone, and polyurethane, have to undergo stringent tests before their
actual use in medical applications (Majumdar, 1998). As compared to other materials the mechanical processing of the polymers
required much less energy (Rosato et al., 2001; Abeykoon et al., 2014). The extrusion process is mainly used for conversion of raw
polymer grains into usable rod or wire form. For reinforcement of ceramic or metal particles in the polymer matrix, a twin screw
extruder (TSE) has been generally used (Erdmenger, 1964). TSEs have numerous advantages over single-screw extruders like better
feeding and more positive conveying characteristics, i.e., they allow the machine to process hard-to-feed materials (Wendaal,
2014). Some studies highlighted that the synthetic hydroxyapatite (HAp) particles were reinforced into a polymer matrix to
produce composites for medical applications and corotating twin-screw compounding produces an effective and homogeneous
distribution of HAp particles in a polymer matrix, which is maintained after compression molding (Wright, 2016; Ben-Gal, 2005;
Wang et al., 1994).
These polymer filaments can be easily used in biomedical applications with the help of additive manufacturing (AM). The
traditional way of implant fabrication has been replaced with AM, in which the implants have been directly fabricated from the 3D
computer aided design (CAD) data (Kurtzman, 2010). Nowadays, AM and CAD have been directly integrated with the 3D imaging
techniques, i.e., magnetic resonance imaging (MRI), computed tomography (CT) scan, etc. (Tukuru et al., 2008). In AM, functional
and nonfunctional prototypes of the polymers have been fabricated by continuously adding layer by layer of material until the
digital CAD model has been completely converted into real time 3D object (Huang et al., 2015). During the past decade a number
of patents have been claimed by inventing vivid types of AM technologies and thus enabling more and more users to install 3D
printers to produce functional products (Wohlers and Caffrey, 2013; Korpela et al., 2013; Zein et al., 2002). The scope of AM is
continuously increasing for biomedical applications with the combination of natural and synthetic polymers by reinforcement of
ceramics, metals, and other foreign particles in these polymers (Seitz et al., 2005).
Fused deposition modeling (FDM) is one of the most widely used AM techniques for fabrication of 3D scaffolds having adequate
mechanical, thermal, as well as surface properties for proper implant placement (Galantucci et al., 2009; Sood et al., 2009). FDM
produces the best fit biofunctional parts in very short duration without the wastage material. FDM uses the 3D CAD model to
fabricate the actual product. Initially the CAD created file is converted into the STereoLithography (STL) format, i.e., machine
language, by using a preprocessing software (Boschetto et al., 2013; Singh et al., 2016, 2017). The .stl file has been further sliced into
2D layers by using an open source software K-Slicer (Chua et al., 2010). The filament has been extruded through the extrusion head
having temperature near the melting point of the material. The temperature of the chamber remains constant to prevent the
solidifying material from thermal stress and distortion. The main advantage of FDM over other AM techniques are its trouble free
handling, and providing controllable factors that have been adjusted according to the required properties of the fabricated part
(Sahebrao et al., 2009). The controllable parameters of FDM affect the various properties of the extruded products (Singh et al., 2016).
In this present work effort has been made to develop the 3D scaffolds on FDM using in-house developed biocompatible
filament comprising of PVC, PP, and HAp (as a case study for field scientists). Initially five input parameters (namely, composition
of material, rpm of the screw, temperature, grain size of HAp, and load applied) were judicially selected for preparation of feed
stock filament. The process parameters of the TSE have been optimized. The wire having best mechanical and dimensional
properties has been run on the FDM setup. The experimentation has been designed using Taguchi L9 (3̂ 3) orthogonal array (OA).
The design of experiment (DOE) has been made on controllable parameters: (1) infill percentage, (2) layer thickness, and (3)
deposition speed. The standard tensile specimen has been fabricated on commercial low cost FDM setup without change in any
hardware or software of the system.
2 Screw Extrusion
Extrusion is a manufacturing process in which metal or plastic materials are forced/pushed through a fixed cross-sectional profile
or die to produce a continuous ribbon of the formed product, or, extrusion is a manufacturing process in which raw materials
(plastic/metal) are melted and made into continual profile.
The extrusion process is starting by feeding of material (metal/plastic) in the form of granules, pellets, powders, or flakes from a
hopper into the zone of the barrel of the extruder. After that, materials are gradually melted by heat produced by the mechanical
energy (generated by screw turning) and by the heaters that are positioned along the barrel. The molten materials (plastic/metal)
are pushed/forced into a die, which structure the materials into a pipe and hardened during the cooling process.
2.2 TSE
The TSE process was developed more than 20 years ago, for continuous production of highly uniform and finely structured
products. It is widely used to produce biosourced plastics, cellulose pulps, and food products. Fig. 3 shows the schematic diagram
of twin screw extrusion (TSE) process.
The main aim of TSE processing is to mix two or more materials homogeneously and produce a very high quality shaped
product with accurate control of process conditions (see Table 1). TSEs are capable of ensuring mixing, shearing, cooling, heating,
Four-Dimensional Printing for Clinical Dentistry 3
Continuous screw
extruder
Non-
Intermeshing
intermeshing
screws
screws
Parallel Conical
screws screws
compressing, transporting, shaping, pumping, etc. with very high level of flexibility. The main advantages of TSEs (intermeshing
corotating) are their exceptional mixing capability that gives remarkable characteristics to extruded products. In the TSE process,
the raw materials may be solids (granules, powders, flours), slurries, liquids, and possibly gases. Table 1 shows the effects of TSE on
different criteria.
4 Four-Dimensional Printing for Clinical Dentistry
Fig. 4 Fused deposition modeling (FDM) process. Reproduced from: CustomPartNet. Available at: www.custompart.net.
3 FDM
In 1988, FDM was invented in the United States by a cofounder of Stratasys Ltd. FDM was patented in 1992 as a rapid prototyping
technology. Commercially FDM is marketed by Stratasys Inc.
Nowadays FDM is a well-known additive technology used for the fabrication of actual or non-actual prototypes. Similar to other
RP technology, it is also a manufacturing tool that produces the part by stacking the material in a layer by layer technique. It is
commonly used for pattern making, modeling, and various production applications. Fig. 4 shows the complete view of FDM process.
Thermal behavior of the material is one of the major constraints for the use of developed filament in clinical dentistry. For thermal
testing of the material in the present study differential scanning calorimetry (DSC) has been used. The term DSC simply implies
that during a linear temperature ramp, quantitative calorimetric information can be obtained on the sample. This constantly rising
temperature ensures the proper and accurate measurement of thermal characteristics of the material. The materials exhibit
heat flow as a function of temperature and time. DSC comprises of glass transition, melting point, enthalpy change, and
decomposition of the material with respect to the rising of temperature. Common usage includes investigation, selection, com-
parison, and end-use performance evaluation of materials in research, quality control, and production applications.
For thermal analysis METTLER TOLEDO, Model DSC3, Swiss make with STARe (SW 14.00) software was used in N2 gas
environment. The typical DSC setup determines the behavior of applied samples by taking references from standard sample, both
enclosed in a metallic crucible (Al or platinum). As shown in Fig. 5, DSC sensor uses two crucibles for heating and cooling, one for
reference and another for sample.
5 Case Study
To study the influences of input process parameters such as barrel temperature, rpm, and applied load on mechanical, thermal,
and metallurgical properties (peak load, peak strength, Young’s modulus, wear analysis, percentage porosity, and shore-D
hardness), a case study has been performed.
5.1.3 HAp
It is also known as hydroxyl apatite. It naturally occurs from calcium apatite.
The chemical formula of HAp (is Ca10(PO4)6(OH)2 or Ca5(PO4)3(OH)4.
Tenacity: brittle.
HAp can synthesize by various methods such as wet chemical deposition, electrodeposition, and biomimetic deposition. HAp
can also synthesize from waste eggshells, which contain 95% calcium. The wet chemical deposition uses the following reaction for
synthesis of HAp.
10CaðOHÞ2 þ 6H3 PO4 -Ca10 ðPO4 Þ6 ðOHÞ2 þ 18H2 O
HAp is available in different colors like white, gray, yellowish, etc. It is brittle in nature. The decomposition range of HAp is
1000–15001C.
In the human body, it is found in bones and teeth. It has been scientifically proven that human bones are constituent 50% by
volume and 70% by weight of hydroxyl apatite.
5.2 Experimentation
In pilot experimentation, an effort has been made to prepare the feed stock filament of biocompatible grade of PVC and PP in the
ratio of 70:30 (by weight). The first step was to check the possibility of preparation of feed stock filament of PVC and PP, which is
further reinforced with HAp with varying input parameters. Taking random selection of different composition/proportions of
polymer materials, the best parametric condition or range of parametric condition was established for TSE. Fig. 8 shows 3D view of
TSE. For this study commercial make HAAKE Mini CTW, Germany has been used.
The feed stock filament has been prepared as per Taguchi L18 (2̂ 1 3̂ 4) OA. Table 2 shows list of input parameters and their
levels (based upon pilot experimentation) for the experimental study.
Table 3 shows the control log of experimentation based upon Taguchi L18 (2̂ 1 3̂ 4) OA, which was 18 runs of experimentation.
Levels Composition of materials Rotational speed Temperature Grain size of hydroxyapatite Load (in kg)
(in percentage) (in rpm) (in 1C) (HAp) (in mm)
1 96A þ 4 30 180 53 10
2 92A þ 8 40 190 106 15
3 – 50 200 150 20
Parametric conditions - Composition of materials Rotational speed Temperature Grain size of hydroxyapatite Load (in kg)
(in percentage) (in rpm) (in 1C) (HAp) (in mm)
1 96A þ 4 30 180 53 10
2 96A þ 4 30 190 106 15
3 96A þ 4 30 200 150 20
4 96A þ 4 40 180 53 15
5 96A þ 4 40 190 106 20
6 96A þ 4 40 200 150 10
7 96A þ 4 50 180 106 10
8 96A þ 4 50 190 150 15
9 96A þ 4 50 200 53 20
10 92A þ 8 30 180 150 20
11 92A þ 8 30 190 53 10
12 92A þ 8 30 200 106 15
13 92A þ 8 40 180 106 20
14 92A þ 8 40 190 150 10
15 92A þ 8 40 200 53 15
16 92A þ 8 50 180 150 15
17 92A þ 8 50 190 53 20
18 92A þ 8 50 200 106 10
For the investigation of mechanical properties, tensile test has been performed for peak load, break load, and Young’s modulus
on universal tensile tester (UTT, Shanta Engineering, India). After establishing mechanical properties the feed stock filament
extruded at best settings has been investigated for thermal properties on DSC setup and metallurgical properties (grain size and
porosity) were observed on metallurgical microscope.
Further for analyzing the dimensional variations, dimensional accuracy (feed stock filament diameter) was measured with
Mitutoyo’s absolute digimatic micrometers. A total of 18 sets of feed stock filament have been prepared by using different con-
trollable parameters (see Fig. 9) and total of 54 (18 3) experiments were conducted to reduce the effect of experimental errors.
8 Four-Dimensional Printing for Clinical Dentistry
The parametric settings (see Table 4) of TSE, at which the feed stock filament possesses better mechanical, thermal properties,
and dimensional stability, have been used for fabrication of 3D scaffolds on the existing FDM setup (without change in any
hardware or software of the system). Further experimentation has been performed for the parametric optimization of the FDM for
various properties of the fabricated functional prototypes/scaffolds.
After preparing filament wire, it was used on existing FDM setup (3D printer, Make-Divide By Zero, India) shown in Fig. 10(a).
The dumbbell shaped tensile specimens as per ASTM D-638 standard were fabricated. The controllable factors of FDM are layer
thickness, infill density, and deposition speed, though there are other parameters like orientation, wire diameter, humidity, etc.,
but kept constant throughout the experimentation. The temperature of extrusion head was also kept constant according to melting
temperature of material. There are further three levels of each selected factor of FDM, as in the case of infill percentage the parts
were fabricated at low density level, high density level, and at solid condition (available in FDM setup as software option).
Whereas for layer thickness and deposition speed three different ranges were selected as 0.25, 0.30, 0.35 mm, and 33, 35, and
37 mm/s, respectively. The parts fabricated by 3D printing were subjected to mechanical testing, surface roughness, shore-D
hardness and dimensional accuracy and thermal analysis. Fig. 10(b) shows the printing of parts on FDM as per ASTM D-638
standard.
The Taguchi L9 OA has been used to design the complete control log of experimentation and input parameters as shown in
Table 5.
Composition of materials Rotational speed Temperature Grain size of hydroxyapatite (HAp) Load (in kg)
(in percentage) (in rpm) (in 1C) (in micron)
Fig. 10 Fabrication of tensile specimen by fused deposition modeling (FDM) extrusion head. (a) Printing of layers for part fabrication start. (b)
Part printing complete.
1 20 0.25 33
2 20 0.30 35
3 20 0.35 37
4 60 0.25 35
5 60 0.30 37
6 60 0.35 33
7 100 0.25 37
8 100 0.30 33
9 100 0.35 35
Four-Dimensional Printing for Clinical Dentistry 9
Fig. 11 Reinforced fused deposition modeling (FDM) fabricated specimen for testing.
A total of 9 sets of specimen have been prepared by using different controllable parameters (see Fig. 11) and a total of
27 (9 3) experiments were conducted to reduce the effect of environmental and human variations, etc. For dimensional analysis
the dimensions of fabricated specimen were compared with the dimensions of standard specimen/CAD data. The surface
roughness, shore-D hardness have been also performed on the fabricated specimens.
Further, the 3D parts fabricated by FDM were subjected to tensile testing on universal testing machine (UTM) as per ASTM
D-638 (see Fig. 12). A total of three sets of experiments/repetitions were performed for nine settings (as per Taguchi L9 OA) by
using different controllable parameters.
After performing the tensile testing, the part with best mechanical properties was used for thermal analysis on DSC and
microscopic analysis by taking the microphotographs through scanning electron microscope (SEM).
Table 6 Outputs of peak load and Young’s modulus for different parametric condition
Parametric Composition Rotational Temperature Grain size of Load Peak Break Young’s
conditions - of materials speed (rpm) (1C) hydroxyapatite (kg) load (N) load (N) modulus (N/m2)
(percentage) (HAp) (mm)
Fig. 13 Main effect plots for signal-to-noise (S/N) ratios for peak load.
As observed in Fig. 13, S/N ratio decreased with increases of HAp proportion. This may be because of the fact that high
proportion of HAp particles leads to more brittleness as it is basically a ceramic material. The S/N ratio for rotational speed first
decreases as rpm increased, and further increased as the rpm increased. At intermediate value of rpm, the dispersion of HAp
ceramic particles may not be uniform, and gets better at further higher values. In the case of temperature, S/N ratio was increased,
with rise in temperature. This may be because of the fact that at higher temperature better melt flow properties are attained. The S/
N ratio for grain size initially decreased then increased, which may due to better dispersion of HAp particles with smaller size. The
S/N ratio for load is continuously decreased as load is increased, mainly because at high load melt flow properties increase
tremendously. Table 7 shows analysis of variance for S/N ratio for peak load.
As shown in Table 7, percentage error was found to be 8.553%. It shows that the model has a higher degree of accuracy. Further it
was observed that composition of material, rotational speed, and load are the only significant parameters, which contribute 39.86%,
28.68%, and 14.49%, respectively, and temperature and grain size (of HAp) was not significant and have less percentage contribution
of 6.38% and 2.02%, respectively. Based upon Table 7, Table 8 shows the response table for S/N ratio for ranking of input parameters.
Finally the calculated value for peak load is 28.38 N, which is close to the experimentally observed value (see Table 6,
experiment no. 9).
Four-Dimensional Printing for Clinical Dentistry 11
Table 7 Analysis of variance for signal-to-noise (S/N) ratios for peak load
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Table 8 Response table for signal-to-noise (S/N) ratios (larger is better) for peak load
Levels Composition of material Rotational speed Temperature Grain size of hydroxyapatite (HAp) Load
Fig. 14 Main effect plots for signal-to-noise (S/N) ratios for break load.
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Levels Composition of materials Rotational speed Temperature Grain size of hydroxyapatite (HAp) Load
25.01%, and 13.25%, respectively, and temperature and grain size (HAp) were not significant and have less percentage con-
tribution, 3.98% and 0.34%, respectively. Based upon Table 9, Table 10 shows response table for S/N ratio for ranking of input
parameters.
For optimization the following formula based upon Taguchi design has been used:
Zopt ¼ m þ ðmA1 2mÞ þ ðmB3 2mÞ þ ðmC3 2mÞ þ ðmD3 2mÞ þ ðmE1 2mÞ
where “m” is the overall mean of S/N data, mA1 is the mean of S/N data for composition of materials at level 1 and mB3 is the mean
of S/N data for rotational speed at level 3, mC3 is the mean of S/N data for temperature at level. mD3 is the mean of S/N data for
grain size of HAp and mE1 is the mean of S/N data for load.
yopt 2 ¼ ð1=10ÞZopt=10 for properties; lesser is betteryopt 2 ¼ ð10ÞZopt=10 for properties; larger is better
Calculation:
Overall mean of S/N ratio (m) was taken from Minitab software.
m ¼ 24:14
Now from response table of S/N ratio, mA1 ¼ 25.61, mB3 ¼ 24.93, mC3 ¼ 24.73, mD3 ¼ 24.33, and mE3 ¼ 25.15.
From here,
Zopt ¼ 24:14 þ ð25:61 24:14Þ þ ð24:93 24:14Þ þ ð24:73 24:14Þ þ ð24:33 24:14Þ þ ð25:15
Fig. 15 Main effect plots for signal-to-noise (S/N) ratios for Young’s modulus.
Table 11 Analysis of variance for signal-to-noise (S/N) ratios for Young’s modulus
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Table 12 Response table for signal-to-noise (S/N) ratios (larger is better) for Young’s modulus
Levels Composition of materials Rotational speed Temperature Grain size of hydroxyapatite (HAp) Load
The magnified image was put on gray scale and analyzed on the basis of porosity. It was observed that percentage of porosity
was less than 1% (0.78) for run 09 and 1.55% for run 13 according to ASTM B276 using MIAS Photomicrographs commercial
software. Total no. of porosity count in the experimentation run no. 09 was 22 and 42 count in run 13. A lower count of porosity
as well as low percentage of porosity was better as per strength, because more porosity decreases the strength of feed stock filament,
so that the as per result feed stock filament no. 09 with lower count of porosity (22) and less percentage of porosity (0.78%) in
feed stock filament no. 13 with greater count of porosity (42) and percentage porosity was 1.55. Hence, lower count of porosity
was better feed stock filament as compared to greater count of porosity. The presence of greater count of porosity in feed stock
filament prepared at run 13, tensile strength was less as compared to lower count of porosity in the best feed stock filament (run
9), which justifies the use of parametric settings suggested for run 9 (as per Table 6).
Fig. 16 Photomicrograph view (for porosity result) for run 9 and run 13.
The S/N ratio plot for shore-D hardness values at larger is best is shown in Fig. 18. The S/N graph shows that with the increase
of HAp percentage shore-D hardness of the parts has been decreased due to increment of brittleness. The S/N ratio for rotational
speed increased as the rpm increased due to proper mixing of polymers with filler. In the temperature S/N ratio first decreases as
temperature increased and further increased as the temperature increased. The S/N ratio of grain size is also continuously increased
with increment of grain size of HAp due to better dispersion of HAp particles. In the load S/N ratio is also increased as the load
increased due to better flow rate.
Analysis of variance of S/N ratios for shore-D hardness shows that two input parameters have been found to be significant
parameters (see Table 14). Rotational speed and composition of materials contribute 67.36% and 15.89%, respectively, toward the
shore-D hardness.
It has been observed that a major effect on shore-D hardness is of rotational speed and composition of materials and there are
much lower effects of temperature, grain size (HAp), and load. Table 15 shows response table for ranking of input parameters
based upon S/N ratio for shore-D hardness.
For optimization following formula based upon Taguchi design has been used:
Zopt ¼ m þ ðmA1 2mÞ þ ðmB3 2mÞ þ ðmC1 2mÞ þ ðmD3 2mÞ þ ðmE3 2mÞ
where “m” is the overall mean of S/N data, mA1is the mean of S/N data for composition of materials at level 1 and mB3 is the mean
of S/N data for rotational speed at level 3, mC1 is the mean of S/N data for temperature at level. mD3 is the mean of S/N data for
Four-Dimensional Printing for Clinical Dentistry 15
Parametric Composition of Rotational Temperature Grain size of Load Shore-D Shore-D Shore-D Shore-D Signal-to-
conditions materials speed (1C) hydroxyapatite (kg) hardness hardness hardness hardness noise (S/N)
- (percentage) (rpm) (HAp) (mm) 1 2 3 mean ratio
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
16 Four-Dimensional Printing for Clinical Dentistry
Levels Composition of materials Rotational speed Temperature Grain size of hydroxyapatite (HAp) Load
Table 16 Dimensional analysis of feed stock filament for different parametric condition
1 1.66 1.62 1.58 1.69 1.74 1.76 1.67 1.54 1.66 1 0.685 0.507
2 1.74 1.71 1.77 1.68 1.48 1.58 1.71 1.79 1.68 3 0.477 0.257
3 1.80 1.89 1.76 1.70 1.67 1.69 1.76 1.55 1.73 4 0.539 0.097
4 1.81 1.75 1.70 1.68 1.73 1.82 1.59 1.66 1.72 2 0.577 0.150
5 1.70 1.68 1.55 1.59 1.74 1.53 1.70 1.73 1.65 0 0.439 0.342
6 1.96 1.84 1.76 1.68 1.82 1.67 1.76 1.68 1.77 5 0.445 0.076
7 1.69 1.64 1.72 1.71 1.55 1.67 1.62 1.52 1.64 0 0.577 0.508
8 1.79 1.75 1.76 1.81 1.67 1.71 1.61 1.57 1.71 3 0.783 0.259
9 1.67 1.64 1.68 1.62 1.63 1.67 1.66 1.63 1.65 0 1.495 1.196
10 1.72 1.73 1.62 1.69 1.51 1.49 1.56 1.63 1.62 1 0.621 0.590
11 1.67 1.62 1.61 1.43 1.48 1.40 1.67 1.69 1.57 3 0.498 0.284
12 1.82 1.89 1.78 1.72 1.59 1.71 1.59 1.68 1.72 3 0.470 0.103
13 1.59 1.49 1.56 1.53 1.62 1.60 1.64 1.63 1.61 1 0.914 0.603
14 1.65 1.47 1.59 1.53 1.69 1.73 1.58 1.64 1.61 1 0.427 0.376
15 1.72 1.71 1.59 1.67 1.53 1.77 1.51 1.65 1.64 1 0.332 0.282
16 1.63 1.68 1.73 1.76 1.67 1.53 1.59 1.61 1.65 1 0.748 0.598
17 1.69 1.61 1.62 1.63 1.56 1.59 1.58 1.61 1.61 0 1.371 1.220
18 1.77 1.81 1.84 1.67 1.74 1.87 1.77 1.73 177 5 0.567 0.113
grain size of HAp and mE3 is the mean of S/N data for load.
yopt2 ¼ ð1=10ÞZopt=10 for properties; lesser is betteryopt2 ¼ ð10ÞZopt=10 for properties; larger is better
Calculation:
Overall mean of S/N ratio (m) was taken from Minitab software.
m ¼ 29:30
Now from response table of S/N ratio, mA1 ¼ 29.87, mB3 ¼ 30.76, mC3 ¼ 29.48, mD3 ¼ 29.63, and mE3 ¼ 29.46.
From here,
Zopt ¼ 29:30 þ ð29:87 29:30Þ þ ð30:76 29:30Þ þ ð29:48 29:30Þ þ ð29:63 29:30Þ þ ð29:46 29:30ÞZopt ¼ 31:82 db
for use in industry for mass production. In the experiment, run no. 17 is good for industry use but because of low tensile strength
feed stock filament is not usable. Fig. 19 shows the dimensional analysis of experiment run no. 09 by using Process Capability
Wizard software.
Fig. 19 Dimensional analysis of experiment runs no. 09 by using Process Capability Wizard. (a) Histogram of experiment run no. 09. (b) Normal
probability plot for experiment run no. 09.
Table 17 Thermal analysis of feed stock filament for different parametric condition
Melting peak (1C) Solidification peak (1C) Melting peak (1C) Solidification peak (1C)
Exp. no. Parameter (A) Parameter (B) Parameter (C) Ra1 Ra2 Ra3 Ra avg. Signal-to-noise (S/N) value (db)
it can be ascertained that in the first and second cycle all the peaks (melting peak, solidification peak) are not disturbed. Therefore
it can be presumed that feed stock filament wire will not lose its properties in the heating and cooling cycle so one can reuse this
filament (after little processing). Fig. 20 shows the thermal analysis of feed stock filament runs 9.
As shown in Fig. 20, for thermal analysis two heating/cooling cycles are involved. In the first cycle, initially heat the sample with
comparison to reference from 30 to 2201C at the rate of 10 K/min, after that in the presence of N2 gas (flow rate is 50.0 mL/min)
cooling process is done in which matter was cooled from 220 to 301C at the rate of 10 K/min. After that in the second cycle,
the same process was repeated. The maximum temperature is taken as 2201C because the material was burnt near 2301C and
lower temperature is generally taken as near to room temperature. It has been observed that peak melting point temperature (Tm)
of run 9 was 160.291C and peak solidification temperature at 116.451C in first cycle and 155.81 and 115.351C in second cycle,
respectively.
The main effect plot for S/N ratio obtained at smaller the better conditions is shown in Fig. 21.
As shown in Fig. 21, with the increase of infill percentage from low density to solid condition the surface roughness decreases.
This may be due to less spacing between the layers of parts. In case of layer thickness with the increase of layer thickness the surface
roughness increases, which may be due to higher amplitude of peaks and valleys at higher value of layer thickness. The deposition
speed does not enroll much effect on the surface roughness as it lies near around the mean line. As shown in Table 3 it has been
observed that the parametric conditions at experiment no. 7 were better for surface roughness.
Analysis of variance has been performed at 95% confidence level for Ra values (see Table 19). The percentage error was found to
be less than 1%, which supports the higher degree of accuracy in the optimization process. Two input parameters were found to be
significant for Ra values, which are infill percentage and layer thickness. As “P” value is not less than 0.05 for deposition speed, so it
was not taken as a significant factor.
Table 20 shows response table for S/N ratio at smaller is better type case, which suggests that the infill percentage has maximum
contribution and deposition speed has minimum effect on Ra. The calculated value for Ra was 4.44 mm, which is very close to the
observed value for experiment no. 7 (see Table 18).
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Table 20 Response table for signal-to-noise (S/N) ratio (smaller is better) for Ra
Levels A B C
Table 21 Control log of experimentations and hardness values with signal-to-noise (S/N) ratios
Exp. no. Parameter (A) Parameter (B) Parameter (C) Shore-D Shore-D Shore-D Shore-D S/N value
hardness 1 hardness 2 hardness 3 hardness avg. (db)
The S/N ratio plot for shore-D hardness values at larger is best is shown in Fig. 23. The S/N graph shows that with the increase
of infill percentage from minimum to maximum density level the shore-D hardness of the parts has been increased. Maximum
hardness is achieved in fully solid parts compared to less dense. In case of layer thickness when it was increased from 0.25 to 0.35
the shore-D hardness decreases, which may be due to the presence of hollow space between more thickened layers. The deposition
speed remains around the mean value and has negligible effect on the shore-D hardness of the fabricated parts.
Analysis of variance of S/N ratios for shore-D hardness shows that two input parameters have been found significant at 95%
confidence level (see Table 23). Infill percentage has more than 95% contribution toward the shore-D hardness. The deposition
speed has been found insignificant due to its “P” value more than 0.05 (Table 22).
Four-Dimensional Printing for Clinical Dentistry 21
Table 22 Analysis of variance for signal-to-noise (S/N) ratios for shore-D hardness
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Levels A B C
Exp. no. Parameter (A) Parameter (B) Parameter (C) DD1 DD2 DD3 DD avg. Signal-to-noise (S/N) values (db)
It has been observed that a major effect on shore-D hardness is of infill density and there is much less effect of layer thickness
and deposition speed. The optimized calculated value for shore-D hardness was 58.922, which was very close to the observed
value in experiment no. 7 (see Table 21). Table 23 shows response table for ranking of input parameters based upon S/N ratio for
shore-D hardness.
Fig. 24 Main effect plot for signal-to-noise (S/N) ratio for dimensional variation.
Table 25 Analysis of variance for signal-to-noise (S/N) ratios for dimensional variation
Abbreviations: Adj. MS, adjacent mean of squares; Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Levels A B C
The response table for S/N ratios at smaller is better type case (see Table 26) suggests that deposition speed has major effect on the
dimensional accuracy of the parts. The calculated value for DD is 0.10, which is the same as observed in experiment run 8 (see Table 24).
Exp. no. Parameter (A) Parameter (B) Parameter (C) Peak load (N) Break load (N)
Based on the values of Table 27, peak load and break load have been optimized by using MINITAB-17 and S/N response was
analyzed to investigate the effect of input parameters at “larger is better” option. The UTM (Shanta Engineering, India) has been
used for tensile testing of the specimens with load cell of 10 KN.
Abbreviations: Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Table 29 Response table for ranking of input parameters for larger is better type case
Levels A B C
Abbreviations: Adj. SS, adjacent sum of square; DF, degree of freedom; F, fishers value; P, probability; Seq. SS, sum of square.
Table 31 Response table for ranking of input parameters for larger is better type case
Levels A B C
where “m” is the overall mean of S/N data, mA3 is the mean of S/N data for infill density at level 3 and mB1 is the mean of S/N data
for layer thickness at level 1, and mC2 is the mean of S/N data for deposition speed at level 2.
yopt2 ¼ ð1=10ÞZopt =10 for properties; lesser is betteryopt2 ¼ ð10ÞZopt =10 for properties; greater is better
Overall mean of S/N ratio (m) was taken from Minitab software. m ¼ 36.58.
Now from response table of S/N ratio, mA3 ¼ 41.94, mB1 ¼ 37.98, and mC3 ¼ 36.82.
Zopt ¼ 36:58 þ ð41:94 36:58Þ þ ð37:98 36:58Þ þ ð36:82 36:58Þ:
6 Conclusions
This study initially highlights the best setting of input parameters of TSE for preparation of in-house feed stock filament based
upon mechanical, thermal, and dimensional properties. The feed stock filament extruded at best settings of TSE have been used to
run in the FDM. Further the parametric optimization of FDM has been also performed for mechanical thermal, dimensional, and
metallurgical properties of the 3D scaffolds with capabilities of 4D features (possible cell growth). Following are the conclusions in
brief of this research study:
• The material composition as 96% polymer matrix (comprising of 70% of PVC and 30% of PP) and filler (HAp) as 4% with
grain size 53 mm at 2001C and rotational speed 50 rpm with load applied of 20 kg were the best conditions observed.
• The results are also supported by microstructure analysis. A biocompatible FDM filament comprising of HAp, PVC, and PP has
been successfully developed with the help of TSE, which has been further used on FDM at various parametric settings without
any change in hardware/software of the system and can be successfully used for preparation of biocompatible dentures in
clinical dentistry with functionally graded tailor made properties.
• The standard tensile specimen (as per ASTM D-638) has been prepared on the different process specific parameters of FDM
with in-house prepared FDM filament comprising of HAp, PP, and PVC, which ensures that the proposed polymer matrix
composite can be successfully extruded for any given mechanical shape.
• The study suggests that with the increase in infill percentage from low density to medium density and further toward the solid,
the surface roughness of the parts has been decreased and shore-D hardness has been increased with the increase of density. But
Four-Dimensional Printing for Clinical Dentistry 27
infill percentage does not have much effect on the dimensional accuracy of the parts. It has been found that the best part has
been fabricated at 100% density level.
• Further the effect of layer thickness has been successfully investigated. The optimized properties have been obtained at
0.25 mm layer thickness. If layer thickness was increased to 0.30 and 0.35 the surface roughness has been increased and
shore-D hardness decreases, respectively. Layer thickness does not show much effect on the dimensional properties of the
reinforced parts.
• It has been found that deposition speed has not shown much effect on the surface roughness and shore-D hardness, but it
majorly affects the dimensional accuracy of the parts. If deposition speed is increased, it decreases the dimensional accuracy.
The best dimensional accuracy has been obtained at 33 mm/s deposition speed.
• It has been observed that when the infill percentage has been increased from low density to medium density and further toward
the solid, peak load values of the specimen have been increased from 31.21 N (specimen no. 3) to 142.29 N (specimen no. 7).
Break load value has been also increased with the increase of density. These are in line with the observations made by other
investigators (Onwubolu and Rayegani, 2014; Carneiro et al., 2015).
• The effect of layer thickness has been successfully investigated. The best results have been obtained at 0.25 mm layer thickness.
If layer thickness was increased to 0.30 and 0.35 the load bearing capacity has been decreased. Both the peak load and break
load values have been decreased with the increase of layer thickness. It has been found that deposition speed has not shown
much attention toward the mechanical properties of the FDM fabricated specimen.
• The thermal analysis using DSC confirms that the samples prepared are thermally stable especially for joining application in
clinical dentistry for job type production activities.
• The microphotographs obtained from the SEM shows that the specimens fabricated by FDM are having open porous and
fibrous structure, which increases the cell cultivation rate for regeneration of new tissues inside the body. Since the functional
prototypes are having porous and fibrous structure, they can be successfully used in clinical dentistry.
Acknowledgment
The authors are highly thankful to Manufacturing Research Lab (Production Engineering Department, GNDEC Ludhiana), DST
(GoI) for financial support to carry out the research work.
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