Universidad Politécnica de Valencia. José Manuel Catalá Civera.

1. “Tecnología Microondas para el desarrollo de Materiales Avanzados”
Prof. Jose Manuel Catalá Civera
Microwave Division, Itaca Research Institute

2.  Microwave Division, ITACA Research Institute, UPV2
CPI
 The CPI brings together the entire l+D+I system of the UPV
• Information and communication technologies
• Health care, life and education
• Nanotechnology, food health and safety
• Transport and automobile industry
• Graphic design and Industrial design
• Energy
• Etc.
 The ITACA Institute is a research and development entity of the Universitat
Politècnica de València,
 Main areas: Digital Electronic systems, Electronics and Sensors, High Performance
Computing Systems, Telecommunication Systems, ICT systems in Health care and
Electromagnetism.

3.  Microwave Division, ITACA Research Institute, UPV3
Microwave Division (DiMaS)
 The Microwave Division (DiMaS) of the research institute ITACA undertakes
scientific and applied research, technological development and technology transfer
initiatives in the field of microwave engineering. DiMaS also offers consultancy
services of advice, high frequency measurements, and expert feasibility studies in
projects of technological development, applicable to the microwave sector.
 Research lines: Numerical techniques & modeling, Design of microwave and RF
techniques, Microwave measurement techniques, Microwave non-destructive
testing (Microwave sensors), Microwave heating.

4.  Microwave Division, ITACA Research Institute, UPV4
Research Lines
 The main research areas in which we focus our activity are:
• Numerical techniques & modeling • Design of microwave & RF circuits
• High power microwave heating
• Microwave measurement techniques.
• Microwave non-destructive testing

5.  Microwave Division, ITACA Research Institute, UPV5
Research Lines
 High power microwave heating. This line develops microwave applicators for
microwave heating in the industry. The design and simulation of the microwave
structure with the processed material, prior to manufacturing, is essential to achieve
all the potential advantages of microwave processing.
Hybrid microwave furnace for high temperature
sintering in controlled atmosphere.
High power microwave heating at ISM frequencies (915 MHz, 2.45 GHz, 5.8 GHz)

6.  Microwave Division, ITACA Research Institute, UPV6
High Power Microwave Heating
 The microwave processing of materials is a relatively new technology that provides
new approaches to improve the physical properties of materials; provides
alternatives for processing materials that are difficult to process.
 Reduces the environmental impact of materials processing; provides economic
advantages through the saving of energy, space, and time; provides an opportunity
to produce new materials and microstructures that cannot be achieved by other
methods.
 Microwave processing is an unusual technology. It is widely used (more than 60
million home units are used to cook food) in an environment in which the user
understands little of the technology.
 Yet, the difficulty in applying the technique in industrial processing has often lead to
frustration of technically competent materials processors.

7.  Microwave Division, ITACA Research Institute, UPV7
What are microwaves?
 The microwaves are electromagnetic radiation and the frequency range lies
between 1 and 300 GHz, and these microwave frequencies with different
wavelengths are used for a wide variety of applications (shown in the Figure). The
domestic microwave applicators work on a frequency of 2.45 GHz. The frequencies
reserved by International Commission for heating purposes in industrial, scientific,
and medical systems are 915 MHz, 2.45 GHz, 5.8 GHz and 28 GHz.

8.  Microwave Division, ITACA Research Institute, UPV8
Heating phenomenon’s of Microwaves
 The heating phenomenon's are different for conventional and microwave
processing of materials.
 Conventional processing methods involve heating of the surface and then
transferring heat into the materials by the phenomenon of conduction, convention,
and radiations; whereas in microwave heating, the atomic level heating is present,
which gives volumetric heating in the processed component. During microwave
heating, the electromagnetic energy gets converted into heat from within the
material, which moves toward the outer direction from the core/center of materials.

9.  Microwave Division, ITACA Research Institute, UPV9
Historical developments showing applications of
microwaves in various fields.
 In recent years, the utilization of
microwaves in various applications has
increased many folds.
 The various processing domains where
this technology has been applied
successfully is shown in the Figure, which
includes communication systems, food
processing, wood drying, enhanced
chemical reactions, vulcanization of
rubber, processing of ceramics and
metallic materials, steel making, joining of
materials, welding, waste treatment, and
recovery of alternate sources of energy.

10.  Microwave Division, ITACA Research Institute, UPV10
Microwave Applications
 Ceramics
 Polymers and Polymer-matrix composites
 Plasma
 Minerals processing
 Microwave Chemistry
 Waste Processing and Recycling
 Examples (powder materials): Sol-gel Decomposition/Drying, Solution
Evaporation/Decomposition, Gas-Phase Reactions, Gas-Solid Reactions, Solid-
State Reactions, Ceramic Precursor Pyrolysis, Hydrothermal Reactions, Powder
Treatment, Dissolution, Drying, Calcining, Powder Consolidation/Shaping,
Sintering, Reaction and Sintering, Melting, Ignition, etc…

11.  Microwave Division, ITACA Research Institute, UPV11
i.e. Microwave Sintering of Ceramics
 Nearly full sintering of Al2O3-based nanocomposites using microwave process
have been achieved much faster and at lower temperature than the conventional
process [1].
R. Benavente, et al., “Fast route to obtain Al2O3-based nanocomposites
employing graphene oxide: Synthesis and Sintering”. Materials Research
Bulletin, Vol. 64, Jan. 2015, pp. 245-251
R. Benavente et al, “Microwave, spark plasma and conventional sintering
to obtain controlled thermal expansion beta-eucryptite materials”.
International Journal of Applied Ceramic Technology, 2014, pp. 1-7.

12.  Microwave Division, ITACA Research Institute, UPV12
High Power Microwave Heating
 The use of microwaves in industrial materials processing can provide a versatile
tool to process many types of materials under a wide range of conditions.
“The ultrafast microwave interaction with materials can create new reaction
pathways and processes not possible using other heating methods”
 Microwave processing is complex and multidisciplinary in nature and involves a
wide range of electromagnetic equipment design and materials variables, many of
which change significantly with temperature.
 A high degree of technical and other (e.g., economic) knowledge is required in
determining how, when, and where to use microwaves most effectively, and when
not to use them.
 Exploiting the potential of microwave processing requires a deep understanding of
the underlying chemo-physical processes at molecular level. A comprehensive
understanding of these correlations requires new and complex instruments and
advanced measurement capabilities.

13.  Microwave Division, ITACA Research Institute, UPV13
Microwave measurement techniques
 New and complex instruments and advanced measurement capabilities. In situ
monitoring ultra-fast microwave heating processes (i.e.chemical reactions, phase
transformation, microstructural evolution, etc).
Fig. 1. Microwave reactor for in-situ monitoring of
microwave heating processes (*)
Experimental set-up.
•Microwave heating reactor
•Calorimetry
•Thermal image
•Video camera
•IR thermometer
•Dielectric properties
•Raman spectroscopy
•Etc.
(*) Jose M. Catala-Civera et al., “Dynamic Measurement of Dielectric Properties of Materials at
High Temperature During Microwave Heating in a Dual Mode Cylindrical Cavity”. IEEE
TRANSACTIONS ON MICROWAVE THEORY AND TECHNIQUES, Vol. 63, 2015, pp. 2905-
2914

14.  Microwave Division, ITACA Research Institute, UPV
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14
Microwave measurement techniques
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Monoclinic Zirconia Tetragonal Zirconia
[1]
[1] Byyung-Kook Kim, Journal
of Materials Science Letters 16
(1997) 669–671
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15.  Microwave Division, ITACA Research Institute, UPV15
Microwave measurement techniques
 Time-resolved X-ray diffraction. The use of high energy synchrotron radiation and fast
X-ray detectors is required for in situ monitoring ultra-fast microwave heating reactions
(i.e. chemical reactions, phase transformation sequences, microstructural evolution,
etc). Pioneering in situ microwave heating experiments using synchrotron radiation are
performed since late 2006 at the Swiss Light Source (PSI, Switzerland).
Fig. 2. Three-dimensional X-ray intensity map
recorded during microwave heating.
Fig 3. Experimental set-up. Reactive synthesis of Ti–Al intermetallics
during microwave heating in an E-field
Fig. 1. In situ TRXRD
synchrotron radiation
experiments are performed at
the Materials Science
beamline MS X04SA .
(*) R. Nicula, et al., “Nanocrystallization of amorphous alloys using
microwaves: In situ time-resolved synchrotron radiation studies”, IOP
Journal of Physics: Conference Series, Vol. 144(12109), 2009, pp. 1-4.

16.  Microwave Division, ITACA Research Institute, UPV16
Research Lines
 Microwave non-destructive testing.(Microwave sensors). This line includes both
basic R&D and applied research in the field of Microwave and Millimeter Wave
Nondestructive Testing and Evaluation. Complete microwave sensors systems are
designed and constructed as portable measurement equipment.
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Dielectric Properties Portable and real
time Measurement equipment (1.5-2.7
GHz)
Microwave sensors for material
properties monitoring
(*) B. García-Baños, et al. “Non-invasive monitoring of polymer curing
reactions by dielectrometry”, IEEE Sensors Journal, Vol. 11(1), 2011, pp
62-70.

17.  Microwave Division, ITACA Research Institute, UPV17
Microwave monitoring & diagnosis
 Microwave curing diagnosis (Correlation with Differential Scanning Calorimetry)
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LOCTITE 9455
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Beatriz García-Baños et al. “Microwave sensor
system for continuous monitoring of adhesives
curing processes”, Measurement Science &
Technology. Vol. 23 (035101), 2012, pp.1-8.

18.  Microwave Division, ITACA Research Institute, UPV18
Research Lines
 Numerical techniques & modeling. This line conducts theoretical research in
numerical methods for the design and modeling of open and closed microwave
structures.

19.  Microwave Division, ITACA Research Institute, UPV19
Example of Numerical Designs
 Numerical techniques & modeling. This line conducts theoretical research in
numerical methods for the design and modeling of open and closed microwave
structures.
Fig.1. Electric Field distribution along the cross
section of the microwave applicator simulated
by QW3D (FDTD)
Dielectric mould (PTFE)
and rubber sample
Collaboration with
Fig 2. Electric Field distribution along
the microwave applicator simulated by
QW3D (FDTD)

20.  Microwave Division, ITACA Research Institute, UPV20
Application Example
 Development of materials with advanced properties by high temperature microwave
sintering. Ultra-light large size mirror (0.5-1 m) with almost zero Thermal Expansion
Coefficient (CTE) for a space optical application .
Manufacturing process
• Blending of positive and
negative CTE materials
• Nanostructuration
• High temperature (>1200ºC)
MW sintering

21.  Microwave Division, ITACA Research Institute, UPV
 High Temperature Microwave Sintering. Microwave sintering has emerged in recent
years as a new method for sintering a variety of materials that has shown
significant advantages against conventional sintering procedures.
21
Application Example
High temperature microwave sintering in a cylindrical
cavity (*)
(*) Rut Benavente et al.,, “Fabrication of near-zero thermal expansion of fully dense β-eucryptite ceramics
by microwave sintering”, Ceramics International , Vol. 40, Issue 1, Part A, January 2014, pp. 935–941.

22.  Microwave Division, ITACA Research Institute, UPV22
Application Example
 New MW-based kiln concepts for with high energy demanding sectors
 From lab-scale to demo pilot plant
 High-quality materials and Energy savings (CO2 reduction)
• High temperature (1500ºC)
• Continuous process
• Adaptive control

23.  Microwave Division, ITACA Research Institute, UPV23
Design of W applicators
 Microwave fuser.
Book on demand (heating paper 5 m/sec).
Fig 2. Paper transport systemFig 1. Heating is divided in 5-7 microwave resonators
WO2008133811 (2008-11-06), “Microwave Fuser apparatus with overlapping heater applications”,
Inventor(s): Rohde D.; Behnke K; Schulze-Hagenest D; Morgenweck F; Catala-Civera J M., Eastman Kodak
Co (USA).

24.  Microwave Division, ITACA Research Institute, UPV24
Design of W applicators
 Continuous Microwave Sintering of Metals/Ceramics
Collaboration with
Fig 1. Electric Field
distribution along the
Microwave Applicator
EP1775998-A1 (2007-04-18), “Microwave-continuous furnace for use during debindering and sintering, has conveying unit directly supported on
body, and microwave-blocking filter arranged at inlet and at outlet of microwave-monomode channel“, Inventor(s): Pueschner P; Catala-Civera J
M, Pueschner Gmbh.

25.  Microwave Division, ITACA Research Institute, UPV25
Design of W applicators
 Combined Microwave Heating
Collaboration with:
Fig 1. Thermograph images of materials
processed with microwaves

26.  Microwave Division, ITACA Research Institute, UPV26
Development of Microwave Processes
Complete engineering support for
development up to demo units
We have more than 20 years addressing
industry heating processes, with more than 25
patents covering the entire spectrum of heating
applications
Design and manufacturing of
new benchtop laboratory
applicators
Including in-situ and real-time control
of the process parameters, optimizing
process efficiency and product quality.
Characterization of materials and
processes
Determination of the material interaction with the
MW fields, getting new or enhanced products,
creating new manufacturing pathways

27.  Microwave Division, ITACA Research Institute, UPV27
Collaborations & Partnership

28.  Microwave Division, ITACA Research Institute, UPV28
Thank you very much for your attention !!!