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Powder Metallurgy

ISSN: 0032-5899 (Print) 1743-2901 (Online) Journal homepage: http://www.tandfonline.com/loi/ypom20

Multiphysic coupling and full cycle simulation of


microwave sintering applied to a ceramic compact
obtained by ceramic injection moulding

J. Shi, Z. Cheng, T. Barriere, B. Liu & J. C. Gelin

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

To link to this article: http://dx.doi.org/10.1080/00325899.2017.1317451

Published online: 01 May 2017.

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POWDER METALLURGY, 2017
https://doi.org/10.1080/00325899.2017.1317451

Multiphysic coupling and full cycle simulation of microwave sintering applied


to a ceramic compact obtained by ceramic injection moulding
J. Shia,b,c, Z. Chengb, T. Barrierec, B. Liub and J. C. Gelinc
a
School of Civil Engineering and Architecture, Southwest University of Science and Technology Mianyang, China; bSchool of Mechanics and
Engineering, Southwest Jiaotong University Chengdu, China; cDepartment of Applied Mechanics, University Bourgogne-Franche-Comté,
COMUE UBFC, Femto-ST Institute, Besançon, France

ABSTRACT ARTICLE HISTORY


Microwave sintering represents the coupling of multiple physical phenomena. It involves the Received 22 February 2016
distribution of electromagnetic fields, heat generation by electromagnetic effects, heat Accepted 4 April 2017
conduction in the material, and evolution of the densification in the sintered components.
KEYWORDS
This paper describes the mathematical models and the numerical methods used to simulate Microwave sintering; powder
the complex sintering process. Simulation results are provided for the prediction of shrinkage compacts; microwave
and evolution of the relative density of the sintered materials. A full cycle simulation of the numerical simulation;
microwave sintering process have been realized on the COMSOL Multiphysics finite element multiphysics; powder
software platform. This work provides an important approach to studying the process of injection moulding
microwave sintering. The simulation results for sintering submicron zirconia powders are
compared with experimental results in terms of the relative densities of the sintered material.

List of symbols microwaves. An area of microwave processing that


E electric field has received a lot of attention is ceramic processing
H magnetic field since ceramics have low thermal conductivities and
mr relative complex permeability are processed at high temperatures. The energy of the
1r relative complex permittivity
1′r dielectric constant microwaves penetrates into the media in the form of
1′′r permittivity electromagnetic waves and results in heating by dielec-
m′′r permeability tric losses. This energy is transformed into molecular
sEC electric conductivity
kinetic energy and then into thermal energy in the
r density
rr relative density materials. Since heat is generated inside the materials,
CP heat capacity together with vibrations caused by the microwaves at
k thermal conductivity high frequency, the temperature of sintered materials
T temperature
P absorbed power density can be increased efficiently. Moreover, the kinetic
tr(1̇) trace of total strain rate energy of molecules and ions in the materials is
1̇ tensor of total strain rate increased by the action of electromagnetic waves.
1̇e elastic strain rate
1̇th thermal strain rate
They also increase the diffusion effect of densification.
1̇vp viscoplastic strain rate These properties are very advantageous for improving
s stress tensor in sintered materials the uniformity of sintered materials at micro and meso
s′ deviatoric stress tensor scales [1]. They exhibit an important potential for uni-
tr s trace of the stress tensor
ss sintering stress form and rapid processing with high production
I second-order identity tensor efficiency [2]. Moreover, microwave heating is selective
GP shear viscosity modulus [3] and generates less pollution [4]; it can be widely
KP bulk viscosity modulus
a coefficient of thermal dilatation used in actual production.
Ee elastic modulus As a combination of the technologies of powder
y Poisson’s ratio metallurgy and microwave heating, microwave sinter-
sair electric conductivity of air
ing has been extensively studied experimentally. Taka-
hashi et al. [5] manufactured a zirconate titanate
1. Introduction
actuator in 2001; Anjana et al. [6] performed research
Research on microwave sintering of powder compacts on Ce2(WO4)3 ceramics at low temperatures. Since
has significant theoretical and industrial value. Heating 1999, after Roy et al. [7] successfully sintered metallic
and sintering by microwaves depends on the sensitivity powder in a microwave field, a wide range of standard
of the response of the sintered materials to the metallic powders have been processed with microwave

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

1′′ r transfer in the material during microwave heating


tan d = . At the macroscopic level, the dielectric
1′ r can be simulated by solving the Fourier’s heat Equation
properties control the microwave processing of a wide (4). This equation couples the distribution of the temp-
range of non-magnetic materials through the quantitat- erature field with the thermal energy generated in the
ive relationship between the absorbed power per unit material. For the ceramic powder compact sample
volume P and the skin depth [20]. Inside the heating exposed to microwaves, this is:
chamber, the volume is divided into two parts: one
∂T
part is the space occupied by the sintered compact, rCP = k∇2 T + P (4)
∂t
and the rest of the space is vacuum, with a different
value of 1r . During the sintering process, electromag- where r is the relative density of the material, CP is the
netic parameters such as 1r and mr etc., are functions specific heat capacity, k is the effective thermal conduc-
of temperature and the relative density of the sintered tivity, T is the temperature and P is a volumetric
powder. The relative density ρ is defined as the ratio source term due to microwave power absorption. Chat-
of the density during sintering divided by the density terjee et al. [22] used the following relation
of the pore-free material. The relative density has a 1 ′
P = v1o 1r E where 10 is the free space permittivity.
strong influence on the heat conductivity and on the 2
electric properties. These parameters are still unknown The thermodynamic parameters such as CP and k
exactly, as research is still needed to calibrate the par- depend on the relative density of the material and its
ameters. In simulations, the reference values of zirconia temperature. Specific experimental measurements are
powder are taken from Santos et al. [21]. still required for calibration of the constants. The
values referenced in the literature are adopted in the
present studies.
2.2. Solve for the distribution of the heat
generation during the process of microwave
sintering
2.4. Solve the governing equations of sintering
The resistance heat generated by the electromagnetic densification to get the structural response of
field or the energy dissipated during microwave heat- the sintered body
ing is the result of absorption of the microwave
The green parts of PIM materials after injection
power in the material [21]. It can be determined by
moulding and debinding consist of porous powders;
Equation (3):
see Figure 1. The densification process during sintering
1 is caused by growth and boundary diffusion of the
P = [(sEC + v1′′r )E2 + vm′′r H 2 ] (3)
2 grains. The mechanical model on a macroscopic scale
where P, sEC and sEC are the absorbed power den- is based on principles of continuum mechanics. An
sity, and the absorbed electric and magnetic fields, analogous viscoplastic constitutive law is adopted to
respectively. sEC is the electric conductivity, describe densification behaviour of the powders. In
1r = 1′r − i1′′r is the angular frequency of the micro- addition, the effects of elasticity and thermal expansion
wave source, and 1′′r and m′′r are the imaginary are taken into account.
parts of the permittivity and permeability of the sin- The sintering process represents the coupling of
tered materials, respectively. several thermo-mechanical phenomena. The densifica-
The present study is focused on the powder of non- tion process of sintered materials is governed by the
magnetic materials. Therefore, the second term on the evolution of the temperature field. It includes the tra-
right hand side of Equation (3) can be neglected [20,21]. ditional governing equations of the mechanical
model, such as the equations for equilibrium and com-
patibility [23]. These traditional equations are not pre-
2.3. Solution of heat transfer equations to sented here. The specific equations for simulation of
compute the temperature field in the sintered the sintering process include the equation of mass
body conservation and the sintering constitutive laws. The
equation of mass conservation takes the form:
In microwave heating, the sintered body is regarded as
a dissipative medium for the transmission of micro- ṙ + r · tr(1̇) = 0 (5)
waves. The dissipation of microwave energy in the where r is density of the sintered material; tr(1̇) is the
medium is treated as a source of the heat, which trace of the total strain rate. The tensor of the total
increases the temperature in the heated body. In the strain rate 1̇ consists of three parts: the elastic strain
heating process, inhomogeneity of the dissipated rate 1̇e , the thermal strain rate 1̇th and the viscoplastic
energy is the result of an uneven distribution of the strain rate 1̇vp .
electromagnetic field. The result is a non-uniform dis-
tribution of the temperature. The process of heat 1̇ = 1̇e + 1̇th + 1̇vp (6)
4 J. SHI ET AL.

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 4. The optimal placement of a ceramic powder of sub-


micronic zirconia particles obtained by the ceramic injection Figure 6. 3D mesh of the ceramic compact for sintering in the
moulding process inside the microwave sintering furnace. COMSOL Multiphysics finite element software.
POWDER METALLURGY 7

Figure 9. Resultant displacement field in the cross section after


Figure 7. Temperature field distribution cross section for
undergoing sintering for 1500 s (case 1: 500 W microwave
500 W microwave power when undergoing sintering for
power).
1500 s with the ceramic behaviour and electromagnetic par-
ameters defined in Table 1. Hatched areas are the sintering
ceramic. simulation for further investigation. The six time
points are chosen to be at equal intervals of the process
density. This cross section is set in a special plane of 1500 s. The peak value of the temperature reaches
located at the middle of the ceramic injection moulding approximately 1650 K near the centre of the sintered
compact, coincident with the symmetry plane (z = compact. The temperature gradient is moderate within
0.134 m plane, filled with slashes, shown in Figure 5). the compact. The temperature in the ceramic becomes
The ceramic powder volume loading after the injec- homogeneous and reaches saturation after approxi-
tion and debinding stages using optimal parameters is mately 1500 s when radiation losses balance the
considered homogeneous using the same methodology absorbed microwave power. The distribution of the
previously developed by Shi et al. [28]. The relative displacement in the horizontal direction at that time
density imposed at the beginning of the sintering and case 1 is shown in Figure 8. The magnitude of
stage is 0.65. The temperature field distribution in the resultant displacement at the same time and case
this cross section, after heating for 1500 s (25 min) 1 is shown in Figure 9. The obvious shrinkage towards
with 500 kW microwave power (case 1), using the cer- the centre and bottom of the compact can be observed,
amic behaviour and electromagnetic parameters which accurately represents the effect of densification.
defined in Table 1, is shown in Figure 7. It represents The final relative density throughout the field is greater
the duration of the entire process of microwave sinter- than 0.9 and can be seen in Figure 10.
ing. The results at six time points are recorded by the

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

of the microwave source, the sintering process can be


controlled to get to a holding stage and then a cooling
stage. For evaluating the simulation result, our exper-
imental results and the experimental results from
Charmond et al. [29] can be used to make compari-
sons. Specimens made using spray-dried 2 mol-%
yttria-doped zirconia nanopowders have been investi-
gated by Charmond and al. [29]. They concluded
that the sintered material showed poor coupling with
the microwaves below 673 K and moderate coupling
above, which agrees well with the simulation result.
With the same maximal sintering temperature of
approximately 1633 K, the corresponding final relative
density using conventional sintering, microwave
sintering and the simulation result can be seen in
Figure 13. Evolution of heat generation during the entire
microwave sintering process. Figure 15. The final relative density is approximately
91.4, 98.6 and 92%, respectively. The result of the simu-
increases continuously with the increase in tempera- lation is slightly lower than the experimental results, as
ture. In the end, the sintered sample can achieve the sintering model for the present simulation is not
near-full densification (relative density greater than precisely calibrated. There is a difference of 7%
92%). The variations discussed can be observed in between the simulation and experimental results. For
Figures 13 and 14. When the power of the microwave some parameters with unknown variability, constant
source is set to a constant value of 1 kW and a fre- values are used in the present simulation. Therefore,
quency of 2.45 GHz, the temperature in the material the simulated evolution of relative density represents
increases continuously. By regulating the input power the use of reference values.

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.

4. Conclusion and outlook His research interests include Prototyping manufacturing


mechanics, simulation of multiphysics fields, modeling of
To simulate the entire microwave sintering process, microwave sintering and injection moulding processes.
modelling of multiple physical phenomena from He is a fellow of the Chinese National Natural Science
microwave heating to densification of the compact Foundation in 2015.
powder has been performed. The process of microwave Z. Cheng is the professor of the Department of Applied
sintering includes coupling the phenomena of electro- Mechanics, Southwest Jiaotong University in China. His
magnetism, heat transfer and sintering densification. main research activity is devoted to the material forming,
the structure safety evaluation and numerical simulation.
Based on an analysis of the principles of microwave Since 2011, having more than 50 papers in national and
sintering, the governing equations which describe the international journal.
three main physical phenomena are provided. Specifi- T. Barriere is a professor of the University Franche-Comté
cally, the constitutive law for sintering behaviour, based and at Femto-ST Institute at the Applied Mechanic Depart-
on previous work of the research team, has been ment, Besancon, France. His main research activity is
implemented into the FE package COMSOL to realise devoted to the material forming process, the powder forming
this coupled multi-phasic simulation. The parameters and the high loaded polymer. Since 2010, having more than
150 papers in national and international conferences.
in the equations have been analysed to identify their
dependence on other factors. The methods used to B. Liu is the professor of the Department of Applied Mech-
anics, Southwest Jiaotong University in China. His main
determine the parameter values are discussed. The
research activity is devoted to the material forming process,
specific configuration of microwave furnace in the lab- the numerical simulation and powder forming process. Since
oratory is taken into account in the simulation. The RF, 1990, having more than 120 papers in national and inter-
heat transfer and structural mechanics modules in the national journal.
COMSOL package have been employed. The constitu- J. C. Gelin is a professor of the Ecole Nationale Supérieure de
tive laws, which describe sintering densification of PIM Mécanique et de Microtechniques, Besançon, France. His
materials at high temperatures, are implemented into main research activity is devoted to the material forming
the structural analysis. Finally, the results of the simu- and micro manufacturing process, the powder forming and
the high loaded polymer. Since 1988, having more than
lation have been analysed. There is a discrepancy of 7% 250 papers in national and international conferences.
between the output of the simulation and the exper-
imental results. This work provides an effective method
for the further analysis and acquisition of knowledge References
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