Thermography of Microsystems

K.-P. Möllmann, N. Lutz, and M. Vollmer, University of Applied Sciences, Brandenburg

Ch. Wille, Clariant GmbH

ABSTRACT
The development and optimization of microsystems, such as microreactors, micro heat exchange systems,
microactuators, microsensors, and others, often require the knowledge of the temperature distribution within
the microsystem. This paper deals with the application of thermography in the 3.5 - 5.5 µm and the 8 -14 µm
spectral bands to such microsystems. The spatial resolution of the temperature measurement was as low as
60 µm, and the time resolution was 20 ms. The results show that this microthermography method is a
powerful tool for the characterization of such microsystems with respect to:
• precise characterization of time-dependent chemical reactions and spatial distribution of the reaction
zone in falling film, glass, and silicon microreactors.
• determination of heat transfer efficiency in micro heat exchange systems.
• characterization of micro Peltier coolers and micro cryogenic actuators.
• characterization of temperature distribution on semiconductor gas sensors.

Keywords: infrared, microsystems, MEMS, spatial and time-resolved thermography

MOTIVATION
Microsystems engineering is likely to be a key technology in the twenty-first century. Microsystems promise to
revolutionize nearly every product category. Light-weight and compact microreactors with increased heat and
mass transfer rates become possible. This results in highly efficient devices for chemical reactions with
extremely precise control of process conditions.
MEMS (micro-electro-mechanical systems) is an enabling technology that allows the development of smart
products, augmenting the computational ability of microelectronics with the perception and control capabilities
of microsensors and microactuators, and expanding the range of possible applications. For a lot of
microsystems, the temperature, the spatial temperature distribution, and thermal response time are among
the most important parameters. Obviously, a contactless measurement is needed to analyze these
parameters for microsystem components (reactors, sensors, actuators). Hence, thermography can play an
important role for the thermal characterization of different microsystems to support research and development
work and to control system operation without modifying system performance.
MICROREACTORS
Falling Film Reactor
DESIGN AND OPERATIONAL PRINCIPLE OF THE FALLING FILM MICROREACTOR
In Figure 1 the components of the falling film microreactor are shown. It can be used, e.g., for gas-liquid
reactions. Figure 1 (right) illustrates the principle to generate thin films in the µm range on a reaction plate
with microchannels. The fluid is distributed on the reaction plate and flows downwards to the withdrawal zone
at the bottom as a fluid film. While the flow direction of the liquid reactant corresponds to the direction of
gravity, the gaseous phase can be guided co- or counter-currently relative to the liquid phase.

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Figure 1. Components of a falling film microreactor (total height 10 cm) and a microstructured reaction plate of falling
film reactor (channel width and depth 300 µm x 100 µm or 1200 µm x 400 µm).
In order to detect the zone of chemical reaction, to measure fluid equipartition and temperature profiles at the
fluid film on the reaction plate, a FLIR® ThermaCam SC 2000 IR camera with a 24° lens was used. To enable
thermal process control, the microreactor was equipped with an IR transparent inspection glass (626 µm thick
Si wafer). In addition, the use of a close-up lens allowed measurements at high spatial resolution (about 200
µm) sufficient to reveal details smaller than the characteristic dimensions of the microreactor.
MONITORING FLUID EQUIPARTITION
In the first experiment on the falling film microreactor, the homogeneity of the microchannels was tested by
studying the wetting behavior of the reaction plate using isopropanol under non-reacting conditions. The
isopropanol film was heated above room temperature to 30°C by an integrated micro heat exchanger. As the
emissivity of the microstructured reaction plate, manufactured in high-alloy stainless steel (ε ≈ 0.5), differs
strongly from that of liquids (ε ≈ 0.9), areas wetted with isopropanol show a bright white color, whereas the dry
areas emit less radiation and show black. This effect was used for easily imaging the fluid equipartition in
parallel channels. In Figure 2 a sequence of the starting wetting behavior at a volume flow of 250 ml/h
isopropanol is shown for a reaction plate with 15 channels at different times.

Figure 2. Starting wetting behavior of a reaction plate with channels 1200 x 400 µm² loaded with a
volume flow of 250 ml/h isopropanol and heated to 31°C at different times.

With respect to the fluid equipartition, the results are in excellent agreement with former investigations [1]. It is
obvious that a very uniform residence time distribution was achieved, since the fluid front has moved the
same distance in all microchannels.

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THERMAL PROCESS CONTROL IN THE FALLING MICROREACTOR

Heat management plays an important role for many reactions. Contactless temperature measurement using
IR cameras enables the recording of a temperature profile of a complete reaction plate, with a single
measurement at high spatial resolution sufficient to reveal details smaller than the characteristic dimensions.
Figure 3 (left) shows an IR image of the temperature distribution of the reaction plate, wetted with isopropanol
under non-reacting conditions while Figure 3 (right) reveals a temperature plot along a line depicted in IR
image, extracted from the corresponding data of the IR image, crossing several microchannels. Apart from
reflection of environmental radiation at the bottom of the reaction plate, the temperature profile is very
homogeneous. The maximum deviation from the set value of 30°C amounts to ± 0.3°C along the line; for the
whole reaction plate area of 27 mm x 65 mm, it amounts to about ± 0.5°C.

Figure 3. IR image with a temperature profile of a heated reaction plate, wetted with isopropanol

MONITORING CHEMICAL REACTION ZONE OF CO2 ABSORPTION IN NAOH(AQ)

The aim of the investigation was to monitor the temperature increase of the liquid phase due to an exothermic
reaction with a gaseous reactant [2, 3]. The investigations were performed in a batchwise manner: the
reaction plate was loaded with a defined liquid flow of NaOH under stationary conditions and an over-
stoichiometric amount of pure CO2 was fed into the gas chamber in counter-flow to the falling film.
The molar concentration of the NaOH solution was 2.0 M, the liquid load of NaOH was 250 ml/h, and the
reaction plate was heated to 25°C by the integrated heat exchanger. In Figure 4 a sequence of IR photos is
provided, illustrating the heat release of a 2.0 M NaOH solution after opening a valve for CO2 supply.
The varying position of the reaction zone within the series of images can be explained as follows: As CO2,
which is heavier than air, is fed in from the bottom into the gas chamber, the reaction front rises as the CO2
level increases in the gas chamber (Fig. 4a - 4d). Complete filling of the gas chamber with CO2 is identified
when the reaction front is leaving the observable area of the reaction plate, and the reaction is quenched at
the bottom (Fig. 4e). At t ≈ 6 s the gas chamber is filled with an excess of CO2. The reaction now only takes
place at the entrance port of NaOH. Then the CO2 supply is stopped. As the CO2 level in the chamber
decreases, the reaction front starts moving downwards again (Fig. 4f, 4g), thereby consuming the remaining
CO2 in the chamber. Whereas the streaming in of the CO2 at the beginning of the experiment is a fast
process, the consumption of it is a slow process of diffusion, showing a broad reaction zone with a small
temperature peak. The CO2 absorption into a 2.0 M solution of NaOH results in a significant temperature
increase of about 1.5°C, which is in the same order of magnitude as calculated data [4].

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Figure 4. Heat release of CO2 absorption into a 2.0 M solution of NaOH. CO2 was fed into the chamber from 0 s to 6 s.
The reaction plate with channels of 1200 x 400 µm² was loaded with 250 ml/h, and the temperature was set to 25°C.
The IR scale corresponds to ∆T=2K from blue to red.

Figure 5. Temperature profile of CO2 absorption into a 2.0 M solution of NaOH from start until complete
consumption of all CO2.

GLASS MICROREACTOR
The Fraunhofer ICT developed a glass microreactor for controlled liquid/liquid chemical reactions with
strongly exothermic behavior [5]. This reactor, shown in Figure 6, is made from photo-etchable, chemical-
resistant, and temperature-stable Foturan® glass.
The reactant liquids are injected through the inputs reactant 1 and 2 (Fig.6). The chemical reaction occurs
within the mixing and the reaction channels (width approximately 120 µm). A separate cooling system is
integrated in the microsystem behind the reaction channels.
Within the wavelength region 3 to 5 µm, the Foturan glass with a thickness of 1 mm shows a transmission of
50%. Therefore, thermal processes inside the reactor can be observed using a short wave IR camera THV
550.

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Figure 6. Micro-glass-reactor (total dimension of the photo 6cm x 8 cm; drain output = blue, reactant 1 input = grey,
reactant 2 input = yellow; cooling system not connected ) for strongly exothermic liquid/liquid reactions.

During the first tests with hot water (T ≈ 80°C), strong temperature inhomogeneities were found (Fig. 7).
These inhomogeneities are amplified during additional cooling with room temperature water. These results
can be used to optimize the assembly of the reacting and the cooling channels.

Figure 7. Test of the microreactor with H2O (80°C) without and with cooling (IR image for ε ≈ 0.9)

As a chemical test reaction, 96% sulfuric acid was diluted with water. Figure 8 demonstrates that time-
dependent, spatially resolved thermography is a powerful method for an adjustment and control of the
process parameters.

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Figure 8. The dilution reaction of 96% sulfuric acid with water occurs in the drain due to unfavorable fluid flow.

If the flow rates and/or the flow rate ratio of the reactants are unfavorably selected, the chemical reaction
occurs not in the microchannels, as desired, but uncontrolled and without necessary cooling within the drain.
These results are used to improve the design of the microreactor to ensure a homogeneous and controlled
chemical reaction inside the reaction channels.

SILICON MICROREACTOR
The silicon microreactor shown in Figure 9 was developed for process-controlled, strongly exothermic
liquid/liquid chemical reactions within 9 parallel microchannels (channel width approximately 300 µm). The
special geometry and the configuration were designed by computer simulations for an optimum mixing of the
reactants. The silicon microreactor should be applied, e.g., for the nitration of diethyl urea with N2O5.

Figure 9: Cutaway view of the Si microreactor and IR image of the reaction channels filled with hot water

The thermography analysis of this nitration reaction of urea results in an unexpected surprise. In contrast to
expectations, inhomogeneous reactions occurred with hot spots along the reaction channels (Fig. 10).
Dependent on the pressure, the flow-rates, and the temperature of the reactants within the reaction zone, the
IR images show time-dependent, localized hot spots like “thunderbolts” in different reaction channels.

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Figure 10. Hot spots due to inhomogeneous reaction

So far, the reasons for these unexpected results are unknown. The structures and the geometries of the
reactor have to be improved in order to get a homogeneous and continuous distribution of the chemical
reaction across the whole reactor.

MICRO HEAT EXCHANGE SYSTEM

The mgt mikroglas technik AG, Germany, has special know-how in the development of microstructured glass
components [6]. One of the latest developments of mikroglas is a micro heat exchanger made from photo-
etchable Foturan glass.
The assembly of the micro heat exchange system is shown in Figure 11. The primary and the secondary
circuits are identical in meander construction. The channels of the primary and the secondary circuits are
directly on top of each other, separated by a Foturan glass plate with a thickness of 200 µm. Both circuits
branch out to 5 meanders with approximately 700 µm channel width.

Figure 11. Assembly of the micro heat exchange system and an IR image of the primary circuit

Applying time- and spatially resolved thermography, the thermal processes and the heat transfer in the micro
heat exchanger can be studied precisely. The different operation methods (co-current and counter-current
flow or parallel and antiparallel mode) can be characterized very accurately (Fig. 12).

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Figure 12. IR image of the primary circuit. Temperature rise of the heat exchanger at co-current flow (top) and
counter-current flow (bottom) after 30 s (left) and 90 s (right). Input (water with T = 60°C) and output of the primary
circuit are marked by red arrows and the cooling water input (T = 25°C) is marked by a blue arrow.

The IR images show a very smoothly varying temperature across the heat exchanger. Due to the small
temperature gradient, system operation is remarkably homogeneous. This is shown in Figure 13. Obviously,
all 5 meanders show about the same temperature gradient, especially for counter-current flow operation.

Figure 13. Temperature profile along selected meanders after ca. 30 s (antiparallel primary and secondary
circuit, noncalibrated temperatures). Meander 1 is partially covered by the housing.

Time-resolved thermography offers the possibility of a detailed analysis of thermal processes, as shown for
counter-current flow in Figure 14. Time-dependent temperatures at selected measuring points can be used to
determine the time response and the heat transfer efficiency. The statistically occurring spikes of temperature
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are caused by small air bubbles within the channels. The apparent temperature change is caused by a
temporary change of emissivity between water and air.

Figure 14. Time-dependent temperatures at selected test points (counter-current flow)

FURTHER APPLICATIONS TO MICROSYSTEMS

Micro Cryogenic Actuators
Cryo grippers from the NAISS GmbH Berlin, Germany [7], are a new patented kind of grippers that form a
connection between the gripper contact surface and the object under study with freezing vapor (Fig. 15). This
method can be used for any hydrophile material. The emerging connection creates a high holding force
without straining the material. Cryo grippers can be used for automatic handling of microprobes, permeable to
air, for non-rigid materials and miniaturized components without any tension force.
Time-resolved thermography appears to be a powerful tool for optimizing the handling process (cooling and
heating). The gripping is based on water vapors in the vicinity of the material. Through an integrated nozzle,
water vapor is sprayed on the gripping spots only. Freezing of the vapor is due to a Peltier cooling element.
This ensures freezing of small amounts of water within a second. The material will be picked up and dropped
off at its destination. For dropping, the frozen vapor, i.e., ice, will be liquefied by heating, which melts the
vapor and dries the material at the same time. The whole task takes only a few seconds.

Figure 15. Photo of the cryogenic actuator and IR image (recorded at an angle from the bottom of the gripper)
during cooling

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Figure 16. Time-dependent temperatures at the cryogenic actuator during cooling and heating

For the optimization and functionality of the gripper, a detailed knowledge of the thermal properties at the top
of the gripper is necessary. Therefore, time-resolved measurements of the temperature distribution were
carried out. Figure 16 shows the temperatures at the top of the gripper during periodic operations of freezing,
transport, and heating. From these, the operating parameters are determined, i.e., the current for the Peltier
cooler/heater at the top of the gripper with regard to the cycle times.

MICRO PELTIER COOLERS

Micro Peltier coolers for spot cooling or temperature stabilization and microthermogenerators are in high
demand for a lot of micro- and opto-electronic applications of the future, due to increasing miniaturization in
these technological fields. Examples are chip cooling in microelectronics or temperature control for
telecommunication lasers. These Peltier coolers and thermogenerators can offer typical advantages of
microsystems, such as short response time and small area, combined with a high thermoelectric energy
conversion. Infineon Technologies AG and Fraunhofer IPM developed the first Peltier devices based on the
V-VI-compounds Bi2Te3 and (Bi,Sb)2Te3, which can be manufactured by means of regular thin film technology
in combination with microsystem technology [8] (Fig. 17).

Figure 17. Miniaturized thermoelectric elements compared to a ‘classical’ Peltier element

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MicroPelt®, the new generation of thermo-electric components, was analyzed by thermography. Some
examples are shown in Figures 18 and 19. Such optimized elements offer a lot of outstanding properties,
such as cooling densities > 100 W/cm2, achievable temperature differences > 40 K, and a time response in
the order of 10 ms [9, 10]. Obviously, contactless IR imaging techniques are extremely useful for time- and
spatially resolved measurements of surface temperatures of these systems.

Figure 18. Photo/IR-image of a MicroPelt® - Peltier cooler

Figure 19. Time response of the miniaturized Peltier cooler from a thermography measurement (applied voltage:
square pulsed = blue curve, step pulsed = red curve)

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SEMICONDUCTOR GAS SENSORS
Gas sensors are of prime industrial interest due to their applications in important fields such as security,
environment, control, automotive, and domestic applications. A particularly interesting class of gas sensors is
based on the resistivity change of metal oxide semiconductor thin films induced by adsorbed gases. The
reversible reactions of adsorption and desorption of different gases are controlled by the operational
temperature (an integrated heater on the chip allows the variation of T between 150oC and 900oC) and the
metal oxides used. Such sensors allow the analysis of various trace gases, such as COx, NOx, NH3, and
hydrocarbons, down to minimum concentrations in the lower ppm range.
During the last decades, mostly thick film devices have been used, although their inherent high power
consumption is undesirable, especially for portable systems. Meanwhile, the technological problems
associated with production of thin film devices have been solved, and the Fraunhofer IPM [11] develops gas
sensor arrays for implementation in commercial systems based on the combination of thin film deposition
techniques, CMOS compatible microfabrication, and bulk silicon micromachining (Fig. 20). There are 4
quadratic gas-sensitive areas with the heater in the centre of the chip.

Figure 20. Photo (chip size approximately 5 mm x 5 mm) and IR image (with an isotherm ∆T = 12 K) of the metal
oxide gas sensors from Fraunhofer IPM

Thermography was used to analyze the surface temperature of the sensors, the thermal response time to
heat up the sensor to the operational temperature, and the spatial temperature distribution on the chip (Fig.
20, 21). The temperature distribution is very homogeneous with ∆T ≈ 10 K.

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Figure 21. Temperature distribution on the chip

The time response during heating is shown in Figure 22. Within a very narrow window, all 4 sensors stay the
same, although their temperatures are continuously rising. The heating process shows two time constants: a
very fast heating up at the beginning and then a slow temperature increase. Because the sensitivity strongly
depends on the sensor temperature, these results are now used to optimize chip structures to get a short-time
response of the gas sensor.

Figure 22. Time-dependent temperatures at sensor areas (SP01-SP04) and the heater (SP05)

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SUMMARY
Thermography is a powerful tool in the development and optimization of a lot of microsystems, such as
micrreactors, micro heat exchange systems, thermoelectric energy conversion systems, microactuators, and
microsensors.

ACKNOWLEDGEMENTS
The authors wish to thank the IMM in Mainz, Germany; the Fraunhofer ICT in Pfinztal, Germany the mgt
mikroglas AG in Mainz, Germany; the NAISS GmbH in Berlin, Germany; and Fraunhofer IPM in Freiburg,
Germany for providing the microsystems used in this work.
This work was partially supported by the applied research grant 17 094 02 from the German Federal Ministry
of Education and Research.

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