To cite this article: J. Shi, Z. Cheng, T. Barriere, B. Liu & J. C. Gelin (2017): Multiphysic coupling
and full cycle simulation of microwave sintering applied to a ceramic compact obtained by ceramic
injection moulding, Powder Metallurgy, DOI: 10.1080/00325899.2017.1317451
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POWDER METALLURGY, 2017
https://doi.org/10.1080/00325899.2017.1317451
CONTACT T. Barriere thierry.barriere@univ-fcomte.fr Department of Applied Mechanics, University Bourgogne-Franche-Comté, COMUE UBFC,
Femto-ST Institute, Besançon, 24 Rue de l’Epitaphe, 25030 Besançon, France
© 2017 Institute of Materials, Minerals and Mining Published by Taylor & Francis on behalf of the Institute
2 J. SHI ET AL.
sintering. The author’s team has long-term experience powders [18] and alumina powders were studied
with powder injection moulding (PIM) and micro-PIM using a conventional sintering furnace [19] by means
technologies, mainly focused on the development of of a dilatometer. A macro model to describe shrinkage
new feedstock formulations [8], modelling and identi- phenomena of the radiatively heated sintering process
fication of physical material parameters [9], a math- was established. These constitutive laws are adopted
ematical model proposed for bi-phase fluid flow [10], in the present paper for modelling of the microwave
and an experimental and numerical analysis of the con- sintering process. A preliminary numerical simulation
ventional thermal sintering process [11]. Furnaces for has also been developed using the finite element solver
microwave sintering have been equipped by the COMSOL Multiphysics. It results in a 3D simulation of
research team for further investigation of the sintering microwave sintering in a multi-mode cavity. The coup-
mechanism by microwave heating. ling of the microwave electric field, thermal conduction
Microwave sintering requires the coupling of and sintering densification of the powdered material is
phenomena from several physical fields. It includes achieved in simulation. To demonstrate possible uses
the coupling of electromagnetic fields, thermal conduc- for the model, a simulation of microwave sintering of
tion and the densification process of sintered powders. submicron zirconia powders is presented.
In a realistic simulation of the microwave sintering
process, these complicated coupling phenomena must
be taken into account. Most of the literature focuses 2. Mathematical model of microwave
on analysis of the microwave heating process. Iskander sintering
et al. used a finite difference method to simulate sinter-
The heating of materials by microwaves is the result of
ing experiments in multi-mode microwave cavities
energy dissipation of the electromagnetic field during
[12]. Campañone et al. [13] developed a simulation
its propagation. To simulate microwave sintering, five
of the heating of foods in microwave ovens. Kozlov
main aspects of the mathematical model must be
et al. [14] proposed and tested simple semi-analytical
established:
models based on a piecewise constant approximation
to the material properties. Shukla et al. [15] compared
the temperature distribution within cylindrical samples 2.1. Solve Maxwell’s equations to determine the
heated in a microwave furnace with those achieved in a electromagnetic fields in the cavity of the
radiatively heated conventional furnace. Kumar et al. furnace
[16] studied the simulation of grain coarsening during
the sintering process. Other papers [12–15] are focused The governing equations of the electromagnetic field at
on macro models that couple microwave heating and a macroscopic scale are Maxwell’s equations. In the
thermal conduction; nevertheless none of them dealt present studies, the fields are affected by the shaped
with the densification process of powder compacts components of non-ferromagnetic or ceramic powders.
during microwave sintering. The heating effect of the magnetic field component of a
As a combination of powder metallurgy and micro- microwave is very small compared to the effect of the
wave heating technology, microwave sintering has been electric field [20]. Therefore, the effect of the magnetic
extensively studied experimentally. With regards to field is not taken into account. The distribution of the
simulation, most of the literature is focused on analysis electric field in the cavity of the furnace can be com-
of the microwave heating process. Macro models that puted by solving Equation (1), as demonstrated in [20]:
couple microwave heating and thermal conduction ∇ × m−1
r (∇ × E) − v 1r E = 0
2
(1)
have been proposed. However, the densification pro-
cess of powdered material during microwave sintering where 1r = 1′r − i1′′r is the relative complex per-
has not been integrated into the simulation of micro- meability, 1r = 1′r − i1′′r is the strength of electric
wave sintering. This process represents the final step field, ω/2π is the excitation frequency of the electromag-
of microwave sintering. The present paper focuses on netic radiation, and 1r = 1′r − i1′′r is the relative com-
the modelling and simulation of the entire microwave plex permittivity, which can be expressed by:
sintering process and on how to introduce the sintering
1r = 1′r − i1′′r (2)
behaviours of sintered powder compact into the simu-
lation. These behaviours present the specific reaction of where 1′r and 1′′r are, respectively, the dielectric constant
sintered material to the microwave heating process. A and dielectric loss factors which quantify the capacitive
mathematical model is established to describe the and conductive components of the dielectric response.
cycle of microwave sintering. Based on a thermo- 1′r is the real part of the dielectric constant, and 1′′r is
elasto-viscoplastic model proposed by Zhang and the imaginary parts of the permittivity, which is an
Gasik [17], a sintering model was developed by Qui- important parameter that determines the dissipation
nard et al. [18] and Song et al. [19]. The sintering beha- of the electric field. Another commonly used term for
viours of compacts formed by 316L stainless steel expressing the dielectric response is the loss tangent,
POWDER METALLURGY 3
Figure 1. Sequential stages for obtaining the final ceramic sintered parts. The sintering stage can be processed using conventional
resistance heating or microwave methods.
The elastic constitutive law for determining the elastic process, which are expressed illustratively by:
strain rate 1̇e and the constitutive law for thermal
a = a(r, T), Ee = Ee (r, T), y = y(r, T) (8)
expansion to determine the thermal strain rate are
the traditional ones [24]. The viscoplastic strain rate where Ee is the elastic modulus of the porous material,
1̇vp and the related constitutive equation, which and y is Poisson’s ratio of the sintered material.
represents the macroscopic response to the sintering
process, is a key requirement for the sintering simu-
lation. By virtue of the model established by Kraft 2.5. Coupling of Maxwell’s equations, the heat
and Riedel [25], the viscoplastic constitutive law for transfer equation and the mechanical equations
the sintering process of powder materials is provided The process of microwave sintering includes three
by Equation (7): types of the physical phenomena. One is the trans-
mission of microwave energy in the heating cavity.
s′ tr s − 3ss Part of the microwave energy is converted into
1̇vp = + I (7) heat energy because of its dissipation during the
2GP 9KP
transmission. The second one is the process of
heat transfer. Because of the uneven distribution of
where s is the stress tensor in sintered materials, s′ is the electric field in the heating cavity, it generates
the deviatoric stress tensor, tr s is trace of the stress heat inhomogeneously in the sintered material as
tensor, ss represents the sintering stress, and I is well. The third one is the densification process
the second-order identity tensor. GP and KP are the during sintering. Particles of the powder and grains
shear and bulk viscosity moduli of the porous of PIM material connect and fuse together while the
material, respectively. GP and KP are determined by pores among the particles are reduced and disappear
means of experimental calibration of the uniaxial vis- gradually, as seen in Figure 1. Macroscopically there
cosity and the viscous Poisson ratio. ss is a function of appears to be shrinkage of the sintered product. The
the apparent density, surface energy and particle sizes. volume is reduced while the density increases. To
It should be calibrated experimentally by sintering the consistently model the sintering phenomenon,
specimens in a dilatometer using different kinetics equations that describe the evolution of the relative
[19]. In the FE simulation for microwave sintering, density and shrinkage must be coupled with the
it is a function of density and the process temperature. electric field and energy balance equations. The evol-
To realise the simulation of the sintering process, ution of relative density and temperature during sin-
the thermal expansion coefficient a for sintered tering results in variability of the different
material, and the material parameters related to elastic parameters in the physical equations during proces-
deformation are required, too. These parameters are a sing. The result is the complicated coupling of
function of density and temperature in the sintering different physics [26].
POWDER METALLURGY 5
Figure 2. The coupling of multiphysics in a full cycle simulation of microwave sintering with COMSOL Multiphysics finite element
software.
3. Numerical simulation of the microwave been carried out for 3D examples with COMSOL
sintering process Multiphysics finite element software. The flow chart
of the coupled multiphysics simulation procedure has
3.1. Model definition
been described, as shown in Figure 2. It includes use
Microwave sintering is the process of realising sintering of the electromagnetism, heat transfer and structure
densification by microwave heating. Modelling the analysis modules along with the implemented sintering
process involves the solution of steady state equations densification module. Coupling of the above-
by frequency domain analysis of the electromagnetic mentioned multiphysics is realised by the functions
fields to determine the distribution of generated heat. of the COMSOL package. These physical phenomena
The temperature distribution in the sintered body is (electric, temperature, displacement fields) are
obtained by a transient simulation of the heat transfer. implemented with tetrahedral elements in the COM-
Evolution of the relative density and shrinkage of the SOL software library. The Petrov–Galerkin method is
PIM material is achieved by mechanical simulation of used to build the procedures for the FEM solution of
the sintering process. the governing equations.
An incremental algorithm is applied for time inte- The cavity of the microwave furnace is regarded as a
gration of the mathematical model, in which the pro- metal box. A microwave source of 2.45 GHz is con-
cesses of microwave sintering of PIM materials are nected with continuously adjustable output power.
described. The governing equations for the three types Two different microwave powers are applied in the
of the above-mentioned physical phenomena are solved studies: input power 500 W for case 1 and input
in fractional steps. In each time step, the distribution of power 1 kW for case 2.
the electric field at that instant is solved by direct As magnetic effects are ignored in the present studies,
methods, while the temperature field and evolution of the microwave source is set to be the transverse electric
the densification is iteratively solved. The coupling (TE) wave. Wall surfaces of the furnace and wave guide
among the three different physical processes is realised are regarded as perfect electrical conductors.
in increments of time steps. In the solution process, The shaped body of the ceramic powder of submi-
the dissipated energy is introduced into the heat transfer cron zirconia particles is modelled in simulation. Refer-
equation (Equation (4)) as an internal heating source. ring to Bouvard et al. [27], its physical parameters are
Then, the distribution of the temperature field is solved shown in Table 1. It should be mentioned that exper-
and introduced into the solution of constitutive equation imental measurements of these parameters are still not
and densification equation. Their solutions define the
evolution of densification and shape deformation during Table 1. The reference physical parameters of zirconia
the full cycle of the sintering process. powder, as shown in [27].
In principle, the electromagnetic and thermal par- Electromagnetic parameters
Air in the cavity: sair = 0, mr air = 1r air = 1;
ameters are not the constants. These material par- Sintered compact: 1r = 10 − i0.1e0.0017(T−293) , mr = 1.
ameters vary as a function of material density and Heat transfer parameters
Thermal conductivity: k = 30rr W m−1 k−1 with rr is relative density;
temperature. The field variables are then solved with Density: r = 6000rr kg m−3;
the updated parameters of the incremental solutions. Heat capacity: CP = 900k J kg−1k−1;
Initial temperature: T0 = 293K.
These cyclic incremental steps run forward until the Densification process
prescribed sintering process is finished. Therefore, Thermal expansion coefficient: a = 1.2 × 10−2 /K;
Poisson’s ratio: y = 0.33;
the simulation process of microwave sintering is the Shear viscosity modulus: GP = 1 × 1011 Pa;
cyclic solutions of Maxwell’s equations, the heat trans- Bulk viscosity modulus KP = 1 × 1011 Pa;
fer equation, as well as the structural equilibrium Initial density: rr0 = 0.65.
Note: Some of the above parameters are the initial ones. For the ones
equation, the material densification equation and the with unknown variation, constant values are taken in the present
constitutive equation. This simulation procedure has simulation.
6 J. SHI ET AL.
Figure 3. Distribution of the electric field in an empty cavity. Figure 5. Geometric dimensions of the ceramic sintered
compact.
all available. The related physical parameters, such as analysed. The result is shown in Figure 3. The sin-
relative permittivity, conductivity, etc., as well as the tered compact should be placed at the position of
analogous viscoplastic constitutive law for sintering of the peak electric field, located in the middle of the
powder compacts, are still current research topics in cavity, as shown in Figure 4. Then, the sintered
materials science. The values retrieved from the litera- material will absorb as much energy as possible
ture represent our limited knowledge. However, the from the microwaves. Geometric dimensions of the
true material parameters are of prime importance for ceramic compact and its 3D mesh representation
accurate simulation of the microwave sintering process. are shown in Figures 5 and 6, respectively.
To simplify the model, it is assumed that the outer
3.2. Results and discussion surface of the sintered compact interacts adiabatically
with the environment in the furnace chamber. For the
The finite element package COMSOL Multiphysics solution of the evolution of heat transfer, the strain–
is employed in the present research. Solutions are stress structural response and relative density, only the
realised using its non-linear solver. Therefore, com- region of the sintered compact is considered in the simu-
putational costs will be reasonable, and half of the lation. Analysis of these effects in the void space of the
geometric model is chosen for the subsequent analy- cavity is not performed because of its unimportance.
sis based on the symmetry of the problem. To deter- The values of important variables in a cross section
mine a suitable position for the sintered compact in inside the sintering compact are investigated to study
the cavity of the microwave furnace, the distribution the evolution of the sintering process. The analysis
of the electric field in an empty cavity is first includes the distribution and variation of temperature,
displacement and the determination of the final relative
Figure 8. Horizontal (x-direction) displacement field in the cer- Figure 10. Final relative density field on the cross section after
amic compact component in the cross section after undergoing undergoing sintering for 1500 s (case 1: 500 W microwave
sintering for 1500 s (case 1: 500 W microwave power). power).
8 J. SHI ET AL.
Table 2. The resultant relative density (D) and sintering temperature (T ) versus time during the
whole sintering process with input power 1 kW and 500 W.
Figure 11. Distributions of final relative density for two different MW sintering conditions: (left) 500 W input power (case 1), sinter-
ing process 1500 s , integrated final relative density 92%. right) 1 kW input power (case 2), sintering process 1000 s , integrated final
relative density 91.4%.
As shown in Table 2, the durations for whole sin- time 1500 s to finish the whole sintering process.
tering process are not the same for different input The disctibutions of final relative density forcases 1
powers. The higher input power leads to more and 2 are shown in Figure 11. The result of simu-
energy absorption, greater heating rate, and then it lation for case 1, with lower heating rate, shows
shortens the whole sintering time. For the case 2 higher final relative density.
with 1 kW input power, the whole sintering time is The 3D shrinkage from debinded to sintered com-
about 900 s to reach the highest relative density for ponents is shown in Figure 12 for both cases 1 and
the prescribed sintering conditions. While for the case 2. Because of the slight difference, one figure is
case 1 with 500 W input power, it needs longer used to illustrate two similar cases. For both the two
sintering conditions, the integrated volume shrinkage
is about of 6–7%.
With the microwave sintering kinetics that were
imposed, the sintering temperature reaches nearly to
the melting point of submicron zirconia powder. The
sintering process is then controlled to run with the suit-
able cycles. The result is a product with nearly full den-
sities that have been achieved in the experiments. Since
the relative permittivity of the material is a function of
temperature, the dielectric loss factor increases with the
increase of temperature. Therefore, generation of
resistance heat in the material is very small in the initial
stages of microwave heating. In the first 10 min, there
is no obvious variation in temperature and relative
density in the material. After 10 min, the temperature
Figure 12. 3D shrinkage from debinded to sintered com- increases at a strong rate in the PIM material as it
ponent, illustration for both case 1 and case 2. reaches its peak value. The relative density also
POWDER METALLURGY 9
Figure 14. Evolution of the relative density vs. temperature and time during the entire microwave sintering process.
Figure 15. The experimental and the numerical results for relative density in conventional sintering and microwave sintering when
undergoing the same heating process to the peak sintering temperature of approximately 1633 K.
10 J. SHI ET AL.
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