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Materials and Design 135 (2017) 26–36

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Adaptive metamaterials by functionally graded 4D printing


M. Bodaghi, A.R. Damanpack, W.H. Liao ⁎
Smart Materials and Structures Laboratory, Department of Mechanical and Automation Engineering, The Chinese University of Hong Kong, Shatin, N.T., Hong Kong, China

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Fabricating adaptive metamaterials by


functionally graded 4D printing tech-
nology
• Building performance-driven function-
ality directly into SMPs by FDM
• Designing adaptive metamaterials by
self-folding/coiling capabilities
• Characterizing self-folding in terms of
printing-speed and liquefier-temperature
• Developing FEM simulations with materi-
al and geometric non-linearities

a r t i c l e i n f o a b s t r a c t

Article history: This paper shows how fused decomposition modeling (FDM) as a three-dimensional (3D) printing technology
Received 20 July 2017 can engineer adaptive metamaterials with performance-driven functionality built directly into materials. The tac-
Received in revised form 26 August 2017 tic is based on an understanding of thermo-mechanics of shape memory polymers (SMP) and fabrication concept
Accepted 30 August 2017
behind FDM as well as experiments to explore how FDM can program self-foldable metamaterials. Self-folding
Available online 1 September 2017
mechanism is investigated in terms of fabrication parameters like printing-speed and liquefier-temperature
Keywords:
that affect layer-by-layer programming process and shape-change. It can be called a functionally graded 4D print-
Material programming ing so that the structure is fabricated additively and programmed functionally. A finite element (FE) formulation
4D printing based on the non-linear Green-Lagrange kinematic relations coupled with a robust SMP constitutive model is
SMPs established to describe material tailoring in fabrication stage and deformation. Governing equations with mate-
Self-folding/coiling rial-geometric non-linearities are solved by implementing iterative Newton-Raphson method to trace large-de-
Experimental demonstration formation non-linear equilibrium path. FDM and FE solution are then applied to digitally design and fabricate
FE analysis straight/curved beams as structural primitives for adaptive metamaterials that show 1D/2D-to-2D/3D shape-
shifting by self-folding or/and self-coiling. Finally, it is experimentally shown that the 4D printed metamaterials
have great potential in mechanical/biomedical applications like structural/dynamical switches, self-conforming
substrates, self-tightening surgical sutures, self-conforming splints and self-coiling/deploying stents.
© 2017 Elsevier Ltd. All rights reserved.

1. Introduction of the epoch [1]. It has drawn considerable attention in scientific/public


community and even allowed anyone to be a designer. 3D printers can
Additive manufacturing (AM), also known as three-dimensional fabricate complex and intricate components with significant reduction
(3D) printing, has been identified as the second industrial revolution in manufacturing time/cost and material wastage. AM techniques avail-
able commercially encompass PolyJet or stereolithography (STL) of a
⁎ Corresponding author. photo-polymer liquid, material extrusion according to ISO/ASTM
E-mail address: whliao@cuhk.edu.hk (W.H. Liao). 52900 [2] or Stratasys fused deposition modeling (FDM) of polymeric

http://dx.doi.org/10.1016/j.matdes.2017.08.069
0264-1275/© 2017 Elsevier Ltd. All rights reserved.
M. Bodaghi et al. / Materials and Design 135 (2017) 26–36 27

filaments and selective laser sintering (SLS) from metallic or polymeric polymers by inducing a compressive strain during photo-polymeriza-
powders. tion in PolyJet process.
Metamaterials as a class of multi-scale structures exhibit thermo- Although it would be straightforward to program 3D printed ob-
mechanical properties that are not found in the nature. Their unusual jects/metamaterials for simple shape change and/or function, it might
characteristics arise from their structure and geometry rather than the be a significant challenge for complicated changes/functions. Further-
matter of which they are composed [3]. In recent years, 3D printing more, it is difficult to perform manipulations needed to program mate-
technology has demonstrated great potential in fabricating metamate- rials manually in certain situations on large or small scales or in remote
rials. For instance, employing Object350 Stratasys 3D printer based on locations such as in space or inside human-body.
the PolyJet technology, Wang et al. [4] introduced dual-material auxetic This paper aims at demonstrating an approach to design and manu-
metamaterials composed of elastic joints and stiff walls without insta- facture adaptive metamaterials enabled by functionally graded (FG) 4D
bility during deformation. Computational results from COMSOL finite printing technology without application of any programming process
element (FE) software and mechanical testing indicated that the dual- and external manipulation. The approach is based on an understanding
material auxetic metamaterial has distinctly different auxeticity and of thermo-mechanics of SMPs and FDM printing technique. Five param-
mechanical properties form traditional single-material auxetic meta- eters as material/surface of platform, its temperature, printing speed,
materials. In another research work [5], they fabricated metamaterials liquefier temperature and delay time for printing each layer are as-
with micro-structured reinforcement embedded in soft polymeric ma- sumed as effective parameters that may influence material tailoring. Ex-
trix. Simulations conducted by ANSYS FE code and uniaxial tension periments are conducted to explore self-folding features in terms of
tests revealed that dual-material designs exhibit strain-stiffening fea- relevant fabrication parameters as well as theoretical framework to de-
tures. Using SLS technology for printing Nylon-based rubber-like mate- scribe phenomena/mechanisms. It is experimentally shown that FDM
rials, Rafsanjani et al. [6] proposed 2D metamaterials that exhibit multi- printing can program SMPs during fabrication in a graded manner for
stability in response to tension. The results from ABAQUS FE and me- desire functions. An FE formulation on the basis of the non-linear
chanical tests revealed that multi-stable responses were triggered by Green-Lagrange strains coupled with a robust SMP constitutive model
snap-through buckling. Mousanezhad et al. [7] investigated 2D auxetic is developed and solved implementing iterative incremental Newton-
metamaterials with structural hierarchy fabricated by Eden260V Raphson technique. It is then applied to explore mechanisms behind
Stratasys 3D printer based on PolyJet technique. Simulations from FG 4D printing and structural shape-change during activation. The
ABAQUS FE code and experiments showed that Poisson's ratio was de- printing method and FE solution are then employed to digitally design
ceased by hierarchy-dependent elastic buckling introduced at early and fabricate self-foldable straight and curved beams as structural prim-
steps of compression. Che et al. [8] proposed methods of small geomet- itives for adaptive metamaterials. The feasibility of 1D/2D-to-2D/3D
ric variations to tune the deformation sequence of 2D metamaterial shape-shifting by self-folding or/and self-coiling features is shown, ex-
with multiple stable states fabricated by PolyJet Object260 3D printer. perimentally and numerically. Finally, some experiments are conducted
There was a good agreement between experimental data and those to demonstrate the potential applications of adaptive metamaterials in
from analytical solutions and ABAQUS FE code. Naddeo et al. [9] pre- mechanical and biomedical engineering devices like structural/dynam-
sented experimental validation of an algorithmic procedure, running ical switches, conformal substrates, surgical sutures, stents and splints.
in ANSYS FE code, able to replace continuous mass of a 3D convex
solid with a cancellous bone-inspired space frame organized for having 2. Concepts and models
fibers oriented according to boundary conditions. A cubic unit cell was
designed and sized to analyze mechanical performances of the new po- The functionally graded 4D printing concept is developed here based
rous material. The numerical results obtained from a unit-cell-based on an understanding of the FDM printing technology and shape memory
analysis were compared with experimental tensile tests on metallic effects. The approach also includes experiments to show its feasibility as
3D printed cubic specimens confirming validity of the beam element- well as a mathematical modeling to describe the mechanism behind it.
based metamaterial. Recently, Bodaghi et al. [10] studied hyper-elastic
behaviors of soft metamaterials fabricated by FDM 3D printing technol- 2.1. FG 4D printing concept
ogy in the large-strain regime experimentally and numerically. Results
revealed that unit-cell shape, direction, type and magnitude of loading The main idea is combination of FDM printing method with SMPs to
had significant influences on anisotropic response of metamaterial create potentials in the design and development of adaptive metamate-
and its instability. rials. SMPs have capacity of retaining a temporary shape and recovering
The 3D printed metamaterials reviewed above all are static and in- to original shape when subjected to environmental stimulus like heat.
animate. Recently, some researchers have employed 3D printing com-
bined with smart materials to offer an innovative method for crafting
active structures [11,12] and metamaterials [12–15]. It is called 4D III
printing where a capacity for movement is latent within the 3D printed
structure. 4D printed structures are able to actively transform configura- IV
tions and evolve over time in response to surrounding stimuli. Among
active materials, shape memory polymers (SMPs) [16–19] and hydro-
philic polymers have been used because of their capability to produce
II
Strain

shape change subjected to an external stimulus such as heat and humid-


ity fields. For instance, Mao et al. [13] introduced a 2D metamaterial lat-
tice with shape-changing feature via printing SMPs and hydrogels by V
PolyJet Objet260. The 4D printed structure expanded by immersing in
water with low and high temperatures, cooling down, drying and then
shrinked upon putting in high-temperature water. Bodaghi et al. [14] I
proposed a self-expanding/shrinking 2D metamaterial lattice by print-
ing fibers of SMPs into flexible matrix using PolyJet Object500 3D print-
er. The metamaterials needed to be programmed through a heating- Temperature
loading-cooling-unloading process after fabrication. Recently, Ding et
al. [15] printed self-foldable metamaterials consisting of stiff and soft Fig. 1. Schematic of the shape memory effect in the strain-temperature plane.
28 M. Bodaghi et al. / Materials and Design 135 (2017) 26–36

Fig. 1 displays a standard step-by-step thermo-mechanical protocol of heated by the hot extruded material when the machine is depositing
programming for SMPs in the framework of a strain-temperature the next layer above them, see Fig. 2. This extra heat definitely affects
phase diagram. It starts at a strain/stress-free state at a low temperature the pre-strain value and reduces it. Therefore, the nozzle temperature
less than transition temperature, T = Tl b Tg, where SMP is stable in a takes account into a significant parameter affecting the pre-strain.
glassy phase. It is then heated above the transition temperature range, Moreover, the temperature of the layer that is being heated is another
T = Th N Tg (step I). Next, SMP stable at rubbery phase is loaded mechan- parameter. This temperature is directly related to the delay time be-
ically to achieve a maximum strain, εm (step II). The strain is kept fixed tween printing each layer. On the other hand, the upper layer as the
and the material is cooled down to the low temperature, Tl, (step III). In end layer never gets any heat since the nozzle leaves it at the end of
this step, the rubbery phase gradually converts to the glassy phase printing stage so that its pre-strain might be the highest one.
memorizing inelastic strains. SMP is finally unloaded while a pre-strain Finally, it can be concluded that printed layers may be programmed
remains in the material, εp (step IV). For the sake of activation, SMP is in different manners and get various values of pre-strain. Also, five pa-
heated to the high temperature, Th, that relaxes strain and recovers rameters as material/surface of platform, its temperature, printing
the permanent shape (step V). This is known as a free-strain recovery. speed, nozzle temperature and delay time for printing each layer can
Now the scope is to implement the above programming protocol dur- be considered as effective parameters that may influence pre-strain
ing printing process. Among various standard 3D printing technologies, values in printed layers. From literature terminology, this printing pro-
FDM technology applies a similar thermo-mechanical procedure on the cess can be called functionally graded 4D printing. The 4D printing pro-
material during fabrication. Fig. 2 displays a schematic of the base of cess could program SMPs during fabrication inducing pre-strain. On the
FDM procedure. The printer performs hot extrusion of a polymeric fila- other hand, this programming could be done in functionally graded
ment through a circular nozzle. The material is heated inside liquefier in manner. While inelastic material property like pre-stain may change
temperature Tln that is above its Tg and then deposited onto the platform layer-by-layer gradually, there are five parameters to control and pro-
by the printer head moving at speed Sp. In fact, the material with high gram the object for desire functions. In this research, FDM printing tech-
temperature is stretched that is similar to the heating-loading process de- nology is implemented to fabricate adaptive metamaterials with
scribed above (steps I and II). After deposition, the printed layer cools and performance-driven functionality built directly into the materials.
solidifies and bonds with the platform that is again similar to the step III in
Fig. 1. Once a layer is completed, the build platform advances downward
2.2. Materials and printing
and printing head proceeds to deposit the next layer. Finally, the thermo-
mechanical programming protocol is completed by mechanical unloading
In this study, polyurethane-based SMP filaments with a diameter of
through removing the printed object from the platform, like step IV.
1.75 mm and glass transition temperature of 60°C is employed (SMP
Therefore, it can be found that FDM has potential to fabricate 3D SMP
Technologies Inc., Tokyo, Japan). All SMP samples are manufactured by
architectures and impose inelastic pre-strain that may drive shape
a New Creator Pro desktop 3D printer developed by FlashForge. New Cre-
memory effects in a prescribed way. In this respect, some printing pa-
ator Pro is a low cost desktop printer that extrudes filaments with a
rameters are supposed to be effective on SMP programming process.
0.4 mm nozzle size. It can be controlled with any open-source software.
For instance, printing speed may have a key role in determining pre-
In this work, Craft-Ware software is utilized to produce G-code files
strain value. It would reasonable that more speed provides more me-
from STL files and to command and control the procedure parameters
chanical loading that may induce more pre-strain, see Fig. 1, step II.
of liquefier temperature and printing speed. As default, liquefier temper-
While all layers are printed with the same printing speed, their surface
ature is set as 230°C while temperatures of build platform and chamber
experiences different thermal/connection conditions. For example,
remain as room temperature, 24°C. Also, the printing speed and layer
while the lower layer, as the first printing layer, is deposited on the
height are set as 20 mm/s and 0.2 mm, respectively. Thermo-mechanical
stiff polymeric printer bed, other layers above it are laid on the already
properties of the printed SMPs are identified by a dynamic-mechanical
printed SMP layers, see Fig. 2. Thus, platform material/surface condi-
analyzer (DMA, NETZSCH, Model 242). To this end, a beam sample is
tions may be important and affect bonding and fixed strain conditions
printed with the dimension of 15 mm (length) × 1.6 mm (width)
in the first layer during cooling and solidifying. Regarding thermal sur-
× 1 mm (thickness). DMA test is carried out in an axial tensile way with
face conditions, temperature of build platform may also affect bonding
frequency of force oscillation 1 Hz and heating rate 5°C/min ranging
conditions and pre-strain value in the first layer deposited on it. Fur-
from −20 to 90°C. Applied dynamic stress to static stress is around 1.5.
thermore, the first layer and layers above it, except the end layer, are
The temperature-dependent results in terms of storage modulus, ES, and
tan (δ) are presented in Fig. 3. As it can be found, the storage modulus
in glassy phase, e.g. in Tl =20°C, is around ESg =1656MPa while it reduces
Liquefier drastically to 3.18MPa at rubbery phase, e.g. in Th =90°C. A high ratio of
storage modulus downfall equal to 520 is observed. Using the formula
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Extrusion nozzle Printing direction for Young's modulus defined as E ¼ ES 1 þ ð tanðδÞÞ2 , Eg = 1657 MPa

Upper layer Molten material


(end layer)
Re-heated zone

Middle layers Solidified material

Lower layer
(first layer)

Build platform
Fig. 3. DMA measurement results for the 3D printed SMP in terms of tan (δ) and storage
Fig. 2. FDM printing process. modulus.
M. Bodaghi et al. / Materials and Design 135 (2017) 26–36 29

and Er =3.26 MPa can be calculated from the DMA test. The prominent
peak in the graph of tan(δ) associated with the glass transition tempera-
ture is read as Tg =60°C. Henceforward, sub-scripts ‘g’ and ‘r’ signify the
glassy and rubbery phases, respectively.
Next, Young's modulus (E), Poisson's ratio (ν) and thermal expan-
sion coefficient (α) of the 3D printed SMPs in glassy and rubbery phases
are specified. To this end, a sample is printed based on the geometry and
dimensions characterized by the ASTM D638 standard [20]. For tensile
tests at low and high temperatures, a Tinius Olsen® H5kS machine
(Tinius Olsen, Horsham, PA, USA) with a 5 kN load-cell and a home-
made thermal chamber is utilized. Material properties extracted from
thermo-mechanical tests are presented in Table 1. The results show
that there is an excellent agreement between measured Young's modu-
lus from DMA and tensile tests. Also, it is observed that, while Poisson's
Fig. 4. Illustration of the 4D printed primitive.
ratio has an increasing trend during phase transformation from glassy to
rubbery, thermal expansion coefficient does not change so that it is the
same at both phases. fact, unbalancing in pre-strain distributed through the thickness leads
a mismatch in free-strain recovery inducing curvatures. It can also be
2.3. Feasibility demonstration concluded that pre-strain may have an increasing trend through the
thickness upward from the lower to the upper layer that may enable
In this section, feasibility of fabricating adaptive SMP metamaterials the overall shape to be changed toward the upper layer. Fig. 5 reveals
by FG 4D printing is demonstrated experimentally. Metamaterials are that printing speed and liquefier temperature have significant effects
designer matter with exotic thermo-mechanical characteristics general- on pre-stain regime through the thickness direction. It is found that
ly adjusted by their architecture rather than their chemical composi- any increase in the liquefier temperature has a negative effect on the
tions. They comprise an arrangement of mechanical elements with pre-strain. This is in accordance with what has been explained in
tunable behaviors. SMP straight and curved beams as structural primi- Section 2.2. The hotter the liquefier, the less the pre-strain. It is also
tives for metamaterials are fabricated by FDM printing method. Geom- seen that enhancing printing speed increases the pre-stain value and
etry and dimensions of a typical printed curved beam with L mean consequently bending deformation. It is reasonable since more speed
length, b width, h thickness, R mean radius and opening angle of θ are provides more mechanical loading that induces more pre-strain, c.f.
shown in Fig. 4. A Cartesian coordinate system (xi, i = 1, 2, 3) is located Fig. 1. Therefore, it can be called a functionally graded 4D printing so
on the mid-plane of the curved beam. Among five parameters that that the structure is fabricated additively and programmed functionally.
may affect pre-strain regime in the 4D printed objects, the effects of Next, it is needed to explore the pre-strain regime in the 4D printed
the printing speed, Sp, and nozzle temperature are examined here. It primitives for enhancing design capabilities.
should be noted that, the nozzle temperature is unknown while tem-
perature of liquefier, Tln, is known and controllable by the Craft-Ware 2.4. Theoretical modeling
software. Therefore, the effect of nozzle temperature is investigated
through temperature of liquefier. Adaptive structures like metamaterials fabricated by FG 4D printing
Four straight 1D beams with L = 15, b = 1.6, h= 1 mm , θ ≅ 0 are fab- method can be designed based on the theoretical understanding of the
ricated by printing parameters of Sp = 30 , 40 mm/s and programming mechanism and thermo-mechanical behaviors of the
Tln = 210 , 230°C as shown in Fig. 5a. The print raster is assumed to be printed elements. This section is dedicated to develop constitutive
along the length direction, x2 direction. In order to activate the printed modeling and mathematical formulation to describe thermo-mechani-
objects, they are heated by immersing into hot water with a prescribed cal mechanisms behind programming in fabrication stage and deforma-
temperature of 90°C that is 30°C more than Tg = 60°C. All the following tion during activation.
samples are also activated by the same method and with the same tem-
perature. The configurations of the elements after hating-cooling pro- 2.4.1. SMP phase transformation
cess are presented in Fig. 5b. Their geometric parameters, L′ , θ′, A robust phenomenological constitutive model basically presented
measured in the x2 − x3 plane are also included in Fig. 5b. in Refs [21,22]. is reformulated here to estimate SMP phase transforma-
The preliminary conclusion drawn from Fig. 5 is this primitive is able tions during thermo-mechanical loadings in a straightforward manner.
to change its configuration over time in the presence of hot water as a SMP materials show a combination of glassy and rubbery features.
heating source. It means they are already programmed and pre-stained The volume fractions of the glassy and rubbery phases are defined as:
during fabrication and are able to react to changes in the environment to
evoke the shape-memory effect. When the primitive printed in the Vg Vr
ηg ¼ ;η ¼ ð1Þ
x1 − x2 plane is exposed to high temperature, it shrinks and bends to V r V
form a curved beam in the x2 − x3 plane and remains folded permanent-
ly, see Fig. 5b. It can be considered as a self-folding 1D-to-2D process where V represents the total volume of the SMP while Vg and Vr are vol-
that may enable pre-designed planar templates to transform into 3D umes of the glassy and rubbery phases, respectively. Since the summa-
structures. This self-bending observed is due to an unbalanced pre- tion of these volume fractions should be unity, i.e. ηg + ηr = 1, the
strain induced during fabrication and deposited along x2 direction. In rubbery volume fraction can be expressed in terms of glassy one as:

ηr ¼ 1−ηg ð2Þ
Table 1
Thermo-mechanical material properties of the 3D printed SMP.
that means there is just one independent volume fraction. As a generally
Parameter Glassy phase Rubbery phase well-known assumption, ηg and Vg are considered to be dependent only
E (MPa) 1660 3.3 on temperature variable, T:
ν 0.35 0.4
α(10−4K−1) 1 1 ηg ¼ ηg ðT Þ; V g ¼ V g ðT Þ ð3Þ
30 M. Bodaghi et al. / Materials and Design 135 (2017) 26–36

Fig. 5. Exprimental illustration on the concept of the functionally graded 4D printing: (a) straight beam printed with different printing speed and liquefier temperature, (b) configuration of
the printed beam after heating-cooling process.

The volume fraction of the glassy phase can be determined accord- in which α is thermal expansion vector and the expression inside the in-
ing to the nature of SMP phase transformation fitting experimental tegral follows the rule of mixture. T0 is also reference temperature.
DMA data. Considering the results presented in Fig. 3, an explicit func- Next, εin that is an unknown quantity is described based on glassy-
tion in terms of trigonometric functions is introduced to interpolate rubbery phase transformation mechanisms. During cooling, the materi-
storage modulus from DMA results as: al is frozen and the rubbery phase changes gradually to the glassy phase.
    In this respect, the strain is assumed to be stocked in the SMP in propor-
tanh a1 T g −a2 T − tanh a1 T g −a2 T h tion to the transformed rubbery phase strain. It is formulated as:
ηg ¼ −     ð4Þ
tanh a1 T g −a2 T h − tanh a1 T g −a2 T l
ε_ in ¼ η_ g εr ð7Þ
in which ai (i = 1, 2) are selected to match DMA curve.
SMP phase transformation occurs by nucleation and growth of plate- where a superposed dot denotes rating function.
let inclusions, mainly directed in the stress direction [21]. Thus, it is con- Regarding the heating, the strain stored is assumed to be released
sidered that glassy and rubbery phases are connected to each other in gradually in proportion to the volume fraction of the glassy phase with re-
series. By considering the fact that the 4D printed objects may experi- spect to the previous glassy phase and stored strain. It is stated as:
ence small strains and moderately large rotations as observed in Fig. 5,
η_ g
a general assumption of additivity of strains is adopted in the form ε_ in ¼ εin ð8Þ
ηg
 
ε ¼ ηg εg þ 1−ηg εr þ εin þ εth ð5Þ
and implies that the strain release is independent of the stress/strain state
during heating.
where ε denotes total strain vector signifying total deformation of the In order to derive stress state, the second law of thermo-dynamics in
material; εg and εr represent elastic strains in the glassy and rubbery the sense of Clausius-Duhem inequality should be fulfilled. By consider-
phases, respectively; εin is associated to inelastic strain due to phase ing ε and T as external control variables, and εg ,εr , εin and ηg as internal
transformations; and εth is called thermal strain and defined as: variables and adopting Helmholtz free energy density functions and fol-
Z T lowing standard arguments, stress quantity, σ, can be derived as:
  
εth ¼ α r þ α g −α r ηg ðT Þ dT ð6Þ
T0 σ ¼ σg ¼ σr ð9Þ
M. Bodaghi et al. / Materials and Design 135 (2017) 26–36 31

in which Heating:

σg ¼ Cg εg ; σr ¼ Cr εr ð10Þ ηg
εin ¼ εkin ð17Þ
ηkg
and C represents elasticity stiffness matrix defined as:
Finally, by considering updated values for inelastic strain, the stress-
2 3
1−ν ν ν 0 0 0 strain relationship (Eq. (12)) can be updated and unified for heating and
6 ν 1−ν ν 0 0 0 7 cooling processes as:
6 7
6 ν ν 1−ν 0 0 0 7
6 ð1−2ν Þ 7  
E 6 0 0 0 0 0 7
C¼ 6 7 σ ¼ Cu ε−β εkin −εth ð18Þ
ð1 þ νÞð1−2ν Þ 6
6
2
ð1−2νÞ
7
7
6 0 0 0 0 0 7
6 2 7
4 5
ð1−2νÞ where Cu and β called unified parameters need to be set for heating and
0 0 0 0 0
2 cooling as:
ð11Þ
8  −1
>
> _
< Cu ¼ I þ Δηg Sr Ce Ce ; β ¼ 1 Tb0
Eq. (9) is consistent with the fact that stress evolutions of each phase ηg ð19Þ
> _
are equal in the series model. : Cu ¼ Ce ; β ¼ ηk
> TN0
g
Next, in order to derive constitutive stress-strain relationship for
SMP materials consists of glassy and rubbery phases, strains from Eq.
(10) are substituted into Eq. (5) that yields: Eq. (18) reveals that the developed constitutive model for SMPs
looks like a linear thermo-elastic model with non-linear material prop-
σ ¼ Ce ðε−εin −εth Þ ð12Þ erties and having inelastic strains known from the preceding time step.

in which 2.4.2. Equilibrium equations


The deformation of the 4D printed objects are expressed in terms of
  −1 the Green-Lagrange strain vector accounted for small strains and mod-
Ce ¼ Sr þ ηg Sg −Sr ð13Þ erately large rotations. The non-linear strain-displacement kinematic
relations can be expressed in a matrix operator form as:
is called an equivalent stiffness matrix and looks like Reuss formula in  
1
the general theory of homogenization. Also, S denotes the compliance ε¼ DL þ DN u ð20Þ
matrix defined as C−1. 2
From a computational point of view, the non-linear SMP behavior
where u indicates generalized displacement vector defined as:
during heating/cooling can be treated as an explicit time-discrete
stress/strain-temperature-driven problem. The time interval [0, t] is 8 9
< u1 =
partitioned into sub-increments and the discretized problem is solved
u ¼ u2 ð21Þ
over a general interval [tk, tk + 1]. For notation simplicity, the variables : ;
u3
with superscript k are associated to the preceding time-step whereas
the ones without superscript are referred to the current step k + 1. It and ui (i = 1, 2, 3) represents displacement components of a generic
is assumed that control variables ε (or σ), T and ηg at time t as well as point within the printed object domain along xi (i = 1, 2, 3) axes,
the solution at time tk are known. The evolution Eqs. (7) and (8) for respectively.
the inelastic strain during cooling/heating can be discretized by implicit Denoting partial differentiation with respect to the spatial coordi-
backward-Euler integration scheme as: nates xi (i = 1,2,3) as:

εin ¼ εkin þ Δηg εr ð14aÞ ∂ ∂ ∂


¼ ∂1 ; ¼ ∂2 ; ¼ ∂3 ð22Þ
∂x1 ∂x2 ∂x3
Δηg
εin ¼ εkin þ εin ð14bÞ DL and DN known as linear and non-linear operator matrices are de-
ηg
fined by:
where 2 3 2 3
∂1 0 0 ∂1 u1 ∂1 ∂1 u2 ∂1 ∂1 u3 ∂1
60 ∂2 07 6 ∂2 u1 ∂2 ∂2 u2 ∂2 ∂2 u3 ∂2 7
6 7 6 7
60 ∂3 7 6 ∂3 u1 ∂3 ∂3 u2 ∂3 ∂3 u3 ∂3 7
Δηg ¼ ηg −ηkg ð15Þ DL ¼ 6
60
0 7; DN ¼ 6 7
6 ∂3 ∂2 7
7
6 ∂2 u1 ∂3 þ ∂3 u1 ∂2
6 ∂2 u2 ∂3 þ ∂3 u2 ∂2 ∂2 u3 ∂3 þ ∂3 u3 ∂2 7
7
4 ∂3 0 ∂1 5 4 ∂1 u1 ∂3 þ ∂3 u1 ∂1 ∂1 u2 ∂3 þ ∂3 u2 ∂1 ∂1 u3 ∂3 þ ∂3 u3 ∂1 5
By using Eqs. (10) and (12) to substitute εr and σ, and preforming ∂2 ∂1 0 ∂1 u1 ∂2 þ ∂2 u1 ∂1 ∂1 u2 ∂2 þ ∂2 u2 ∂1 ∂1 u3 ∂2 þ ∂2 u3 ∂1

some mathematical simplifications, the inelastic strain (Eqs. (14a) and ð23Þ
(14b)) can be updated explicitly for cooling and heating processes in
stress and strain control manners as: It can be shown that variation of strain field is derived as:
Cooling:
δε ¼ ðDL þ DN Þδu ð24Þ
εin ¼ εkin þ Δηg Sr σ for stress control mode ð16aÞ
Equations of equilibrium as well as the corresponding boundary
conditions are derived in a straightforward manner from the principle
 −1  
εin ¼ I þ Δηg Sr Ce εkin þ Δηg Sr Ce ðε−εth Þ for strain control mode
of the minimum total potential energy as:

ð16bÞ δU−δW ¼ 0 ð25Þ


32 M. Bodaghi et al. / Materials and Design 135 (2017) 26–36

in which variations δU of the strain energy and δW of the work done by They all are defined as:
the external loads need to be substituted with their definitions in terms
of stresses, forces, virtual strains and virtual displacements. ðDL ΨÞT Cu ðDL ΨÞT dV
K0 ¼ ∭ V  
Starting from the variation of the strain energy 1
KL ¼ ∭V ðDL ΨÞT Cu ðDN ΨÞT þ ðDN ΨÞT Cu ðDL ΨÞT dV
2
1
δU ¼ ∭V δεT σ dV ð26Þ KN ¼ ∭V ðDN ΨÞT Cu ðDN ΨÞT dV
8 29 8 9
< Q1 = < Q i−1 = ð33Þ
Fm ¼ Q 2 ; Q i ¼ ⋮ ; i ¼ 1; 2; 3
and using stress definition (Eq. (18)), it can be rewritten as: : ; : ;
Q 2 ui−20
  Fkin ¼ β∭ V ðDL ΨÞT þ ðDN ΨÞT Cu εkin dV
δU ¼ ∭ V δεT Cu ε−β εkin −εth dV ð27Þ  
F th ¼ ∭V ðDL ΨÞT þ ðDN ΨÞT Cu εth dV

where V signifies the volume of the printed structure. The potential en- It should be mentioned that, εkin and εth are known variables through
ergy of external loads can be also expressed as: the SMP element that are held into the volumetric integrals. In this re-
spect, T is assumed to be constant through the element volume while
δW ¼ δuT Q ð28Þ the Gauss-Legendre numerical integration method is implemented to
calculate the integral including εkin along xi (i = 1, 2, 3) coordinates. A
3 × 3 ×3 discrete grid Gauss points having 3 points along each xi axis is
where
considered in this study. Finally, in order to construct global FE
8 9 governing equations, Eq. (32) is assembled for all elements that results
< Q1 = in:
Q ¼ Q2 ð29Þ
: ;     
Q3 k
K0 þ KL U þ KN U U ¼ Fm þ Fin þ Fth ð34Þ

denotes point forces in the xi (i = 1,2,3) directions. Eq. (34) represents a non-linear set of equations due to geometrical
non-linearity. Consequently, an iterative solution procedure such as
2.4.3. FE methodology Newton-Raphson technique [23] is implemented to solve the problem
In this division, a Ritz-based FE solution is developed to predict func- in a step-by-step mode. By knowing temperature T, mechanical loading
tionally graded 4D printing process and thermo-mechanical behaviors Fm and inelastic strain field εkin from the previous load-step, new value of
of 4D printed metamaterials. A 20-noded quadratic serendipity hexahe- U is calculated iteratively. Afterwards, the strain and stress state can be
dron element with 3 degrees of freedom (i.e. ui (i =1,2, 3)) per node is computed using Eqs. (30), (20) and (18), respectively. Finally updated
proposed for the present problem. Considering quadrilateral shape inelastic strains at all Gauss points are calculated through either Eqs.
functions ψi(x1, x2, x3) (i = 1…20) [23], the displacement vector u can (16a) and (16b) or (17) for cooling or heating process.
be approximated in terms of nodal-mechanical variables as: It should be noted that, in the printer nozzle, the polymer melt is
under stress, with part of the deformation energy being stored elastical-
u ¼ ΨU ð30Þ ly. As the polymer melt leaves the nozzle, stresses are relaxed and the
elastically stored energy is released, leading to radial expansion of the
in which Ψ and U are elemental interpolating matrix and generalized melt referred to as die swelling. The phenomenon may affect pre-strain
nodal displacement vector defined as: regime induced by 4D printing process. For predicting die swelling and
investigating its effects on pre-strain regime, viscoelastic-based SMP
2 3 constitutive model should be developed, even though it is beyond the
ψ 0 0 objective of the present work. For more details on modeling of visco-
Ψ ¼ 0 ψ 05
4
elasticity in SMPs and die swelling, one may refer to [24–26].
0 0 ψ
ψ ¼ fψ1 ⋯ψ20 g
ð31Þ 3. Adaptive metamaterials: design-fabrication-simulation
0 ¼ f8
0⋯09 g 8 9
< u1 = < ui−1 =
U ¼ u2 ; ui ¼ ⋮ ; i ¼ 1; 2; 3 In this part, the developed computational tool is first implemented
: ; : ;
u3 ui−20 to describe thermo-mechanical mechanisms behind SMP material tai-
loring during fabrication stage. It is then applied to digitally design
primitives fabricated by FG 4D printing for adaptive metamaterials
where ui−j (i = 1…3;j = 1…20) are mechanical nodal variables.
By substituting the discretized displacement field (Eq. (30)) into the
strain field (Eq. (20)) and its variation (Eq. (24)) and subsequent results
into the virtual energies (Eqs. (27) and (28)) and the principle of
minimum total potential energy (Eq. (25)), FE governing equations for
a generic element can be derived as:

ðK0 þ KL ðUÞ þ KN ðUÞÞU ¼ Fm þ Fkin þ Fth ð32Þ

where K0 represents the constant stiffness matrix while KL and KN are


linear and quadratic stiffness matrices which are dependent on the
nodal displacements. Also, Fm , Fkin and Fth are load vectors induced by
mechanical loading, SMP phase transformation and thermal loading
due to temperature change from a reference temperature, respectively. Fig. 6. Model prediction for Young's modulus and comparison with experimental DMA data.
M. Bodaghi et al. / Materials and Design 135 (2017) 26–36 33

Table 2 and Table 2 also reveal that the 4D printing process with parameters
Predictions for pre-strain (%) regime of the SMP beam printed in various printing speeds of Sp = 40 mm/s , Tln = 230°C and Sp = 30 mm/s , Tln = 210°C induces
and liquefier temperatures.
similar pre-strain into the beam structure and results in nearly similar
Location Sp = 30 mm/s Sp = 40 mm/s configuration after activation. Finally, it can be concluded that control
Tln = 210°C Tln = 230°C Tln = 210°C Tln = 230°C of printing speed and liquefier temperature may allow the realization
of self-folding 3D structures. The pre-strain regime and its values re-
Upper layer 30.5 15 37 31.3
Middle layers 25.3 10.1 29 24 ported in Table 2 may serve as benchmark data to researchers dealing
Lower layer 20 5.6 21 17 with design, simulation and fabrication of FG 4D printed object. From
a technical viewpoint, objects printed with high temperatures may
have a strong interface bonding. Therefore, the following results are
that can reveal self-assembly functions. Finally, several 3D adaptive printed with fabrication parameters of Sp = 40mm/s and Tln = 230°C.
metamaterials with shape-shifting features that illustrate broad poten-
tial applications are presented. 3.2. Primitives for adaptive metamaterials

3.1. Pre-strain regime prediction Five 2D primitives with different shapes are proposed for designing
adaptive metamaterials with self-folding feature. First, one straight and
The first step is to predict pre-strain value induced in all printed two curved beams with the same length, width and thickness
layers during fabrication. In order to achieve the investigation, phase- (L = 34, b = 1.6,h = 1 mm) and different angels of θ = 0 , 60 and 90° are
transformation parameters including a1 , a2 , Tl and Th presented in Eq. printed as illustrated in Fig. 7a. The configurations of the primitives
(4) need to be calibrated. Using DMA results already displayed in Fig. after hating-cooling process are displayed in Fig. 7b. The FE model is
3, they are set as 0.15, 0.145 and 20, 100°C, respectively. Young's modu- also implemented to simulate structural deformations using pre-strain
lus calculated from Eq. (13) is illustrated in Fig. 6 and compared with ex- regime reported in Table 2 for Sp = 40 mm/s and Tln = 230°C. Simula-
perimental data from DMA. The results reveal that the trigonometric tions are also included in Fig. 7c. The color bar in Fig. 7c displays trans-
function is able to successfully simulate SMA phase transformation in verse displacement (u1), along X1-direction, to maximum transverse
a smooth and gradual manner as observed in experiments. displacement (u1m). In this aspect, u1m is reported in Fig. 7c. The results
The initial and final status of the straight beams as displayed in Fig. show that, while straight beam has a shape-shifting via self-bending
5 are given as inputs and applied to FE tool. Implementing a try and mechanism, curved beams experience both bending and cross-sectional
error scheme, pre-strain regime in terms of its value at lower, middle rotation at the same time. In fact, once activated by hot water, the free-
and upper layers is computed and presented in Table 2 for various strain recovery stands the curved beam up while natural curvature
printing speeds and liquefier temperatures. As it can be seen, pre- leads the structure to rotate along the length direction. It results in
strain has an almost linearly increasing trend through the thickness forming a conical ring with rectangular cross-section that is oblique
upward inducing self-folding feature. During heating, the pre-strain with respect to the ring axial direction. From a topology point of view,
is released non-uniformly. This un-balancing produces bending defor- in fact, inner and outer edges of the curved beam with small and large
mation and leads to self-folding. In this respect, any increase in print- radii make the apex and base of truncated conical shell-like structures.
ing speed or liquefier temperature has positive and negative effects on Furthermore, it is interesting to note that all beams with the same
the induced pre-strain value and consequently structural deformation length either in curve shape or straight transform to rings with similar
as observed in experiments, see Fig. 5. The results presented in Fig. 5 mean diameters (≅ 7 mm) so that both end edges meet each other.

(a)

(b)

(c)

u1m=0 mm u1m=17.4 mm u1m=22.4 mm

Fig. 7. Straight and curved 4D printed primitives: (a) initial configuration after printing, (b) final configuration after heating-cooling, (c) simulation.
34 M. Bodaghi et al. / Materials and Design 135 (2017) 26–36

Fig. 8. Wave-shaped (a–c) and extended wave-shaped (d–f) 4D printed primitives: (a, d) initial configuration after printing, (b, e) final configuration after heating-cooling, (c, f) simulation.

Their difference is cross-section angle with respect to the ring axial direc- will be required to print some supportive material that may affect surface
tion is measured as 22 and 31° for initial primitives printed with angels of quality and mechanical properties/strengths of the spring.
60 and 90°. Regarding simulation, it is noted that the FE model-solution is It is interesting to note that the helical is permanent shape of the self-
able to correctly replicate main characteristics observed in the experi- coiling structure. It means it is possible to program it into any other
ments. In this aspect, maximum error of 2% is achieved for mean diame- shape as a temporary shape and then achieve free shape recovery upon
ters that is acceptable. It should be mentioned that the simulations have heating. For instance, the spring as depicted in Fig. 9a is heated by im-
been performed using pre-strain information obtained from the previous mersing in hot water with temperature of 90°C and then straightened.
test (Table 2). The good qualitative and quantitative agreement obtained Next, it is kept fixed and cooled down to the room temperature followed
with the same pre-strain for both tests confirms accuracy and reliability by mechanical unloading, see Fig. 9b. It looks like a straight beam with
of the predicted pre-strains in the previous section. 54 mm length. Heating the straightened 1D beam will result in fully
These self-foldable primitives can serve as elements of adaptive shape recovery as shown in Fig. 9.
metamaterials for complicated shape-changes or complex functions. It
is worth mentioning that, while the mass of the printed elements re-
mains constant during phase transformation, the geometry and stiffness
are changed. It means dynamic properties are changed as the 4D printed
object is heated. They could be a good candidate to be employed as
adaptive structural/dynamic switches providing different tempera-
ture-dependent dynamic characteristics. For instance, they may be
promising in designing self-foldable metamaterials for affecting reso-
nance behaviors [27].
Next, another primitive with geometrical parameters of the curved
beam described above with L = 34 , b = 1.6 , h = 1 mm and θ = 60° is
printed in a symmetric wave-shaped form. In fact, it is composed of
two arcs with θ = 30°. The configurations of the sample after printing
and heating-cooling are demonstrated in Fig. 8a and b. Simulations are
also embedded in the third part of the figure. As it can be seen, the 2D
wave-shaped primitive gets into a ring shape but has a derivation along
the circumferential direction. A qualitatively and quantitatively good
agreement between experiment and simulation is also observed. The
final shape looks like a helix of helical spring. It brings the idea that the
planar wave-shaped component may be employed for designing adap-
tive metamaterials in spring shape. The wave shape template is then ex-
tended in both directions to have four segments of arcs with θ=30°. The
counterpart of Fig. 8a–c for the current example is depicted in Fig. 8d–f.
The results reveal that the extended wave-shape template transfers to a
helical spring with two coils after heating-cooling process. It can be a
Fig. 9. Thermo-mechanical programming on the self-coiling spring: (a) initial
demonstration of 2D to 3D shape-shifting by self-coiling mechanism. configuration after printing-heating-cooling process, (b) final configuration after
Thus, it can be called a self-coiling spring. Beyond self-coiling feature, a heating-straightening-cooling-unloading (the straightened beam is recovered back to
static spring could be printed directly by FDM 3D printing. However, it the spring upon heating).
M. Bodaghi et al. / Materials and Design 135 (2017) 26–36 35

Fig. 10. 4D printed self-conforming device: (a) straightened beam and a hex key, (b) conforming to radius of 6.8 mm, (c) configuration after full shape recovery; 4D printed self-tightening
fiber: (d) straightened beam and soft polymeric substrate, (e) forming a loose knot, (f) shrinkage of the fiber by heating.

3.3. Potential applications loosely connected by the 1D straightened beam at room temperature,
see Fig. 10e. When the temperature is increased above the critical tem-
This section is dedicated to demonstrate potential applications of perature, Tg, the adaptive metamaterial is activated triggering the shape
self-folding primitives and self-coiling springs in mechanical and bio- recovery and removes the gap and tighten the tissue-like substrate, see
medical engineering devices. For example, the self-coiling spring dem- Fig. 10f. In fact, it acts like a self-tightening fiber. This may pave the way
onstrated in Fig. 9 can serve as spiral stents. In the straightened shape, for 4D printing patient-design self-tightening fibers for surgical sutures.
the 1D beam can be placed inside a catheter and then delivered to the As a final example, straight beam element presented in Fig. 7 is used
required location. Once the constraint is removed, the 1D beam may to design and fabricate planar metamaterial (34 mm × 17.6mm × 1 mm)
be heated by blood temperature and mechanically self-coil. It may act by self-folding ability. It is composed of a periodic arrangement of the
like a supporting function for opening the artery keeping blood flowing six straight primitives (34 mm × 1.6 mm × 1 mm) programmed along
normally or encompasses any object like a blood clot for treating stroke. their length direction during printing stage as depicted in Fig. 11a.
In the next example, the 1D straightened beam presented in Fig. 9b Upon heating, the 2D lattice transforms to shape a 3D tubular
is used as a 1D element that softens and conforms to 3D environments metamaterial as shown in Fig. 11b. The inner dimeter is also similar to
upon heating. Fig. 10a displays the 1D component and a hex key with that of self-foldable primitive. It confirms reliability of SMP program-
a diagonal of 6.8 mm. The experimental results presented in Fig. 10b ming during FG printing process so that all beam-like elements are
and c reveal that, after warming, the 1D smart component is able to soft- programed in a similar way. This 4D printed planar metamaterial with
ly conform to the 3D hexagonal supporting environment. Even after self-folding capability may has potentials to be used as adaptive cus-
cooling, the device retains its conformed geometry and shape fixing, tom-designed structures that may conform to cylindrical environment
see Fig. 10c. It can be found that this adaptive element has potential to and perform supporting function. It can be used in biomedical devices
be used as flexible and conformal components for future mechanical/ for different supporting usages like broken bones or tracheal splint.
biomedical devices fabricated by 4D printing technology. Motivated by Such a 4D metamaterial may exhibit another great potential to serve
the research work of on shape memory suture [28], the feasibility of as a self-deployable stent, see Fig. 11c and d. To this end, it needs to be
the current 1D-to-3D self-coiling metamaterial for a similar purpose is heated and rolled to get like a smaller cylinder as shown in Fig. 11d. It
checked experimentally. A two-part soft polymeric substrate that is able to retain the temporary shape by fixing-cooling-unloading pro-
looks like tissue, (30 mm × 15 mm × 1 mm) × 2, as shown in Fig. 10d, is cess. The small tube can be stored inside a catheter and then delivered
36 M. Bodaghi et al. / Materials and Design 135 (2017) 26–36

(a) (b) (c) (d)

heating

programming

Fig. 11. 4D printed metamaterial lattice with self-folding capability: (a) after printing, (b) after heating-cooling process; 4D printed self-deploying stent: (c) another view of part b, (d)
configuration after heating-rolling-cooling-unloading (the rolled cylindrical lattice deploys upon heating).

to the required position. Once the catheter is removed, it is heated to [5] K. Wang, C. Wu, Z. Qian, C. Zhang, B. Wang, M.A. Vannan, Dual-material 3D printed
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