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Blockage by Dendritic Ice in Supercooled Encapsulated
Water

JUAN J. MILÓN G., Researcher, Technological Research Laboratory in energy, San Pablo Catholic
University, Arequipa, Perú, milonjj@ucsp.edu.pe
SERGIO L. BRAGA, Researcher, Energy Laboratory, Pontifical Catholic University of Rio de Janeiro. Rio de
Janeiro. Brazil, slbraga@mec.puc-rio.br




ABSTRACT

An experimental device was developed to investigate the blockage by dendritic ice in supercooled water
encapsulated process inside cylindrical capsules used for cold storage process. The coolant is a water-alcohol
mixture (50% vol.), controlled by a constant temperature bath (CTB). Temperatures varying with time are
measured inside and outside the capsule. Cylinder with internal diameter and thickness of 45 mm, 1.5 mm and
length 170 mm, respectively, the capsules were made in acrylic, PVC (polyvinyl chloride), bronze and
aluminium materials. The results indicate that when the supercooling phenomenon appears, the nucleation
process varies according to the temperature distribution of the phase change material, PCM and of the coolant
temperature. It has been observed that when the supercooling phenomenon appears, and later the nucleation, a
blockage by dendritic ice appears. This blockage was classified according to the capsule material and the coolant
temperature, showing different types: total blockage and partial blockage (50% and 25%).


1. INTRODUCTION

    While the water is cooled in an enclosed container, freezing does not occur at its freezing point (0°C) at
atmospheric pressure. Instead, it is normally cooled below 0°C before ice nucleation happens. Supercooled water
refers to a metastable liquid state even though the water temperature is below its freezing temperature. The
metastable state will end when ice nucleation occurs and the thin plate-like crystal of dendritic ice grows into the
supercooled region of water. During the dendritic ice growth process, latent heat is released from the dendritic
ice and consumed by supercooled water. At the end of this initial growth process, normally the temperature of
water returns to its freezing point (0°C). If the metastable state exists and remains during the thermal storage
process, thermal energy can only be stored in the form of sensible energy. In this case, the storage capacity is
strongly reduced. There are several studies about supercooled water. Chen et al. (1998) studied the numerical
and experimental method to analyze the influence of nucleation agents in the water solidification process inside
cylindrical copper capsules of different sizes. Yoon et al. (2001) studied experimentally the freezing
phenomenon of saturated water within the supercooled region in a horizontal cylinder using the holographic real
time interferometry technique. Milón and Braga (2003) studied the phenomenon of supercooling in spherical
capsules of different diameters and determined the parameters that influence this phenomenon appearance.
Milón and Braga (2004) studied the dendritic ice growth in supercooled water inside cylindrical capsule. Gilpin
(1977) studied the dendritic ice form in a pipe during the freezing process. It has been show that growth of
dendritic ice can cause blockage by the water in the pipe.

2. EXPERIMENTAL MODEL

    The experimental apparatus, shown schematically in Figure 1, consists in a test section (a), an observing
system (b), a cooling system (c), and a measurement and data acquisition system (d).
Blockage by Dendritic Ice in Supercooled Water Encapsulated Process




                                      ACQUISITION
                                        SYSTEM
                                          (d)             CTB                UPPER
                                                           (c)             RESERVOIR
                                                                               (c)


                                                                                   TEST
                                                                                  SECTION
                                                                                    (a)

                                              CTB-IC
                                                (c)




                                                                   LOWER
                                                 DIGITAL          RESERVOIR
                                                 CAMERA               (c)
                                                   (b)


      Figure 1 – Experimental apparatus schematic diagram: test section (a); observing system (b); cooling system (c) and
                                         acquisition and measurement system (d)

2.1. Test section.
     This section contains the capsule to be analyzed. The walls are made of 10 mm thick acrylic plate externally
covered with 25 mm thick insulation. A cross section is shown in the Figure 2. The diffuser function is to
homogenize the coolant temperature (TC) in the test section. The temperature control is carried out by a constant
temperature bath which receives the signals from a temperature sensor RTD type PT-100. K type thermocouples
were used for the circulating fluid temperatures registration. Two flanges are installed in the vertical walls to
facilitate the capsule installation. An overflow tank, working at atmospheric pressure, was installed to
compensate the volume variation during the phase change process. In the same figure, the cylindrical capsule,
filled with the PCM (distilled pure water), can be observed. To define the volume of the PCM, a sliding disk
(movable in the axial direction) is used. K type thermocouples of 0,076 mm diameter, covered with Teflon, are
also indicated.

                        NITROGEN                RTD
                                                                 COOLANT
                         OUTLET                PT-100
                                                                                        SECONDARY
                                                                                        DIFFUSER

                                                                                             THERMOCOUPLES
                       FIXED DISK                                   CAPSULE

       DIGITAL
       CAMERA
                                                                                                         OVERFLOW
                                                                                                         TANK
                                                 PCM


                                                                                        SLIDING DISK
                        NITROGEN
                        CHAMBER




                         NITROGEN
                           INLET                                 COOLANT        PRIMARY
                                          THERMOCOUPLES                         DIFFUSER

                                              Figure 2 – Test section details
Blockage by Dendritic Ice in Supercooled Water Encapsulated Process




2.2. Observing system
    A digital camera (30 images per second), located inside an extern container, is used to register the exact
instant of the nucleation and the growth of the dendritics ice (Figure 2). To avoid condensation, the space
between the capsule and the camera’s lens is filled with nitrogen, inert gas that removes the humid air. The box
is also insulated.

2.3. Cooling system
   The cooling system is schematically showed in Figure 1. It is composed by two constant temperature baths
(CTB), two reservoirs (upper and lower) and the coolant. The initial temperature for the tests is set at one
CTB-IC while the other CTB is set at the test temperature. The temperature control system Proportional Integral
Derivative (PID) maintains the temperature into a range of ±0.05 °C with a refrigeration power of 800 W at 0 ºC
and 1000 W of electric power heater. The coolant is an alcohol-water solution (50% in volume).

2.4. Measuring and data logging system
   The measurements and storage of data are made by the data acquisition system and a personal computer
(PC). The acquisition equipment, which communicates with the PC by the RS232 communication port, receives,
processes and transmits the temperature signals to PC, for storage and posterior analysis.

3. EXPERIMENTAL PROCEDURE

    Stage I: The initial water temperature inside the capsule (25.0 ºC) is imposed using the constant temperature
bath for the initial condition (CTB-IC). The other CTB controls the coolant temperature in the upper reservoir.
    Stage II: The coolant of the upper reservoir pass through the tests section imposing the test temperature,
absorbing the initial thermal loads and passing later to the lower reservoir.
Stage III: The coolant of the CTB is addressed toward the test section until the conclusion of the test.
Stage IV: After each test, a pump impels the coolant toward the upper reservoir for a new test.
This procedure is carried out to maintain constant the test temperature along each test. The duration of each test
varies from 30 to 60 minutes, depending of the test conditions. The data is acquired once a second. Uncertainties
are presented in Table 1.

Table 1: Uncertainties of measurements
Parameter                       Uncertainty
Temperature                     0.1 ºC
Time                            0.01 s
Length                          0.01 mm

3.1. Investigated parameters
   The following parameters were investigated: blockage by dendritic ice formation and inside the cylindrical
capsules made of bronze, aluminium, acrylic and PVC. The capsule has a 45 mm internal diameter and 1.5 mm
wall thickness. Experiences were carried out with different temperatures of the coolant (TC= -6, -8, -10, -12, -14,
-16 and -18 ºC). Each experience was done 20 times with the same conditions.

4. RESULTS AND DISCUSSION
    In Figure 3, can be observed the characteristics blockage by dendritic ice in the acrylic capsule with TC = -16
ºC and TC = -12 ºC. When the nucleation happens, according to the temperature distribution of the PCM in the
capsule, two types of blockage by dendritics ice formation appear; the partial blockage and the total blockage.
These differences happened when before the nucleation, the PCM is partially supercooled (partial blockage) or
the PCM is totally supercooled (total blockage). During the nucleation process, the latent heat released by the
dendritics ice and consumed by supercooled water, causing the different blockages.
photographic image         time, s                   photographic image           time, s




                                               0                                                       0




                                               1                                                       1




                                               2                                                       2




                                              2.5                                                     2.5




                                              22.5                                                     6




     Figure 3 – The blockage for dendritic ice growth. Acrylic capsule with TC = -16 ºC (left) and TC = -12 ºC (right)

   The figure 4 represent most of the observed curves (a probability of more than 60%) the blockage for
dendritics ice formation, for different capsule materials and different temperatures of the coolant. It can be
observed, a zone where the phase change process without the dendritic ice formation, classified as zone of steady
processes without supercooling presence. The central area is a blockage’s region, varying according to the
material and the coolant temperature. To the right area presents of the metastable liquid region, the liquid
remains below of Tm, without a nucleation presence.
   In the PVC capsule, the majority of the tests did not present supercooling phenomena (without blockage), the
process of phase change vary rapidly from steady to metaestable liquid process.
Blockage by Dendritic Ice in Supercooled Water Encapsulated Process



                   Bronze


                                        SOLIDIFICATION
                                         STEADY ZONE
                                          (WITH OUT
                   Aluminium




                                        SUPERCOOLING)
capsule material




                                                                               SOLIDIFICATION
                                                                              METASTABLE ZONE
                   Acrylic




                                                                                                                           LIQUID METASTABLE
                                                                            (WITH SUPERCOOLING)
                                                                                                                                  ZONE
                                                                                                                            (WITH PERMANENT
                                                                                                                             SUPERCOOLING)
                   PVC




                                  -18          -16           -14           -12           -10            -8            -6            -4             -2
                                                                             Coolant Temperature, TC, ºC


                                        Total blockage             Partial blockage to 50%             Partial blockage to 25 %


                               Figure 4 – Blockage for dendritic ice for different temperatures of the TF and different materials of the capsule

5. CONCLUSIONS

   The blockage for dendritic ice growth is a function of the coolant temperature and the capsules material. It
can be observed that the presence of total blockage and partial blockage. In the PVC capsule did not present
supercooling phenomena (without blockage). For the dendritic ice formation, necessarily the supercooling
phenomenon must appear.

6. ACKNOWLEDGEMENTS

   This paper was supported by the Conselho Nacional de Desenvolvimento Científico e Tecnológico – CNPq of
Brazil. The authors also wish to thank the Agreement Pontificia Universidade Católica do Rio de Janeiro and
Universidad Católica San Pablo for motivating this research work.

NOMENCLATURE

TC                                   coolant temperature, [ºC]                           CTB-IC        constant temperature bath of initial
PCM                                  phase change material                                             conditions of the PCM
CTB                                  constant temperature bath                           PVC           polyvinyl chloride
Tm                                   freezing temperature

REFERENCES

    Chen, S. L., Lee, T. Z., 1998, A study of supercooling phenomenon and freezing probability of water inside
horizontal cylinders, International Journal of Heat and Mass Transfer 41: (4-5, 3), 769-783.
    Gilpin, R.R., 1977, The effect of cooling rate on the formation of dendritic ice in a pipe whith no main flow.
ASME Journal of Heat Transfer 99: 419-424
    Milón, J.J., Braga, S.L., 2003, Supercooling Water in Cylindrical capsules, Fifteenth Symposium on
Thermophysical Properties, National Institute of Standards and Technology, Colorado, USA.
    Milón, J.J., Braga, S.L., 2004, Dendritic Ice Growth in Supercooled Water Inside Cylindrical Capsule,
International Refrigeration and Air Conditioning Conference at Purdue, USA.
    Yoon, J.J., Moon, C.G., E.Kim, Son, Y. S., Kim, J.D., Kato, T, 2001, Experimental study on freezing of
water with supercooled region in a horizontal cylinder, Applied Thermal Engineering 21Ç 657-668.

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Blockage by Dendritic Ice in Supercooled Encapsulated Water

  • 1. Blockage by Dendritic Ice in Supercooled Encapsulated Water JUAN J. MILÓN G., Researcher, Technological Research Laboratory in energy, San Pablo Catholic University, Arequipa, Perú, milonjj@ucsp.edu.pe SERGIO L. BRAGA, Researcher, Energy Laboratory, Pontifical Catholic University of Rio de Janeiro. Rio de Janeiro. Brazil, slbraga@mec.puc-rio.br ABSTRACT An experimental device was developed to investigate the blockage by dendritic ice in supercooled water encapsulated process inside cylindrical capsules used for cold storage process. The coolant is a water-alcohol mixture (50% vol.), controlled by a constant temperature bath (CTB). Temperatures varying with time are measured inside and outside the capsule. Cylinder with internal diameter and thickness of 45 mm, 1.5 mm and length 170 mm, respectively, the capsules were made in acrylic, PVC (polyvinyl chloride), bronze and aluminium materials. The results indicate that when the supercooling phenomenon appears, the nucleation process varies according to the temperature distribution of the phase change material, PCM and of the coolant temperature. It has been observed that when the supercooling phenomenon appears, and later the nucleation, a blockage by dendritic ice appears. This blockage was classified according to the capsule material and the coolant temperature, showing different types: total blockage and partial blockage (50% and 25%). 1. INTRODUCTION While the water is cooled in an enclosed container, freezing does not occur at its freezing point (0°C) at atmospheric pressure. Instead, it is normally cooled below 0°C before ice nucleation happens. Supercooled water refers to a metastable liquid state even though the water temperature is below its freezing temperature. The metastable state will end when ice nucleation occurs and the thin plate-like crystal of dendritic ice grows into the supercooled region of water. During the dendritic ice growth process, latent heat is released from the dendritic ice and consumed by supercooled water. At the end of this initial growth process, normally the temperature of water returns to its freezing point (0°C). If the metastable state exists and remains during the thermal storage process, thermal energy can only be stored in the form of sensible energy. In this case, the storage capacity is strongly reduced. There are several studies about supercooled water. Chen et al. (1998) studied the numerical and experimental method to analyze the influence of nucleation agents in the water solidification process inside cylindrical copper capsules of different sizes. Yoon et al. (2001) studied experimentally the freezing phenomenon of saturated water within the supercooled region in a horizontal cylinder using the holographic real time interferometry technique. Milón and Braga (2003) studied the phenomenon of supercooling in spherical capsules of different diameters and determined the parameters that influence this phenomenon appearance. Milón and Braga (2004) studied the dendritic ice growth in supercooled water inside cylindrical capsule. Gilpin (1977) studied the dendritic ice form in a pipe during the freezing process. It has been show that growth of dendritic ice can cause blockage by the water in the pipe. 2. EXPERIMENTAL MODEL The experimental apparatus, shown schematically in Figure 1, consists in a test section (a), an observing system (b), a cooling system (c), and a measurement and data acquisition system (d).
  • 2. Blockage by Dendritic Ice in Supercooled Water Encapsulated Process ACQUISITION SYSTEM (d) CTB UPPER (c) RESERVOIR (c) TEST SECTION (a) CTB-IC (c) LOWER DIGITAL RESERVOIR CAMERA (c) (b) Figure 1 – Experimental apparatus schematic diagram: test section (a); observing system (b); cooling system (c) and acquisition and measurement system (d) 2.1. Test section. This section contains the capsule to be analyzed. The walls are made of 10 mm thick acrylic plate externally covered with 25 mm thick insulation. A cross section is shown in the Figure 2. The diffuser function is to homogenize the coolant temperature (TC) in the test section. The temperature control is carried out by a constant temperature bath which receives the signals from a temperature sensor RTD type PT-100. K type thermocouples were used for the circulating fluid temperatures registration. Two flanges are installed in the vertical walls to facilitate the capsule installation. An overflow tank, working at atmospheric pressure, was installed to compensate the volume variation during the phase change process. In the same figure, the cylindrical capsule, filled with the PCM (distilled pure water), can be observed. To define the volume of the PCM, a sliding disk (movable in the axial direction) is used. K type thermocouples of 0,076 mm diameter, covered with Teflon, are also indicated. NITROGEN RTD COOLANT OUTLET PT-100 SECONDARY DIFFUSER THERMOCOUPLES FIXED DISK CAPSULE DIGITAL CAMERA OVERFLOW TANK PCM SLIDING DISK NITROGEN CHAMBER NITROGEN INLET COOLANT PRIMARY THERMOCOUPLES DIFFUSER Figure 2 – Test section details
  • 3. Blockage by Dendritic Ice in Supercooled Water Encapsulated Process 2.2. Observing system A digital camera (30 images per second), located inside an extern container, is used to register the exact instant of the nucleation and the growth of the dendritics ice (Figure 2). To avoid condensation, the space between the capsule and the camera’s lens is filled with nitrogen, inert gas that removes the humid air. The box is also insulated. 2.3. Cooling system The cooling system is schematically showed in Figure 1. It is composed by two constant temperature baths (CTB), two reservoirs (upper and lower) and the coolant. The initial temperature for the tests is set at one CTB-IC while the other CTB is set at the test temperature. The temperature control system Proportional Integral Derivative (PID) maintains the temperature into a range of ±0.05 °C with a refrigeration power of 800 W at 0 ºC and 1000 W of electric power heater. The coolant is an alcohol-water solution (50% in volume). 2.4. Measuring and data logging system The measurements and storage of data are made by the data acquisition system and a personal computer (PC). The acquisition equipment, which communicates with the PC by the RS232 communication port, receives, processes and transmits the temperature signals to PC, for storage and posterior analysis. 3. EXPERIMENTAL PROCEDURE Stage I: The initial water temperature inside the capsule (25.0 ºC) is imposed using the constant temperature bath for the initial condition (CTB-IC). The other CTB controls the coolant temperature in the upper reservoir. Stage II: The coolant of the upper reservoir pass through the tests section imposing the test temperature, absorbing the initial thermal loads and passing later to the lower reservoir. Stage III: The coolant of the CTB is addressed toward the test section until the conclusion of the test. Stage IV: After each test, a pump impels the coolant toward the upper reservoir for a new test. This procedure is carried out to maintain constant the test temperature along each test. The duration of each test varies from 30 to 60 minutes, depending of the test conditions. The data is acquired once a second. Uncertainties are presented in Table 1. Table 1: Uncertainties of measurements Parameter Uncertainty Temperature 0.1 ºC Time 0.01 s Length 0.01 mm 3.1. Investigated parameters The following parameters were investigated: blockage by dendritic ice formation and inside the cylindrical capsules made of bronze, aluminium, acrylic and PVC. The capsule has a 45 mm internal diameter and 1.5 mm wall thickness. Experiences were carried out with different temperatures of the coolant (TC= -6, -8, -10, -12, -14, -16 and -18 ºC). Each experience was done 20 times with the same conditions. 4. RESULTS AND DISCUSSION In Figure 3, can be observed the characteristics blockage by dendritic ice in the acrylic capsule with TC = -16 ºC and TC = -12 ºC. When the nucleation happens, according to the temperature distribution of the PCM in the capsule, two types of blockage by dendritics ice formation appear; the partial blockage and the total blockage. These differences happened when before the nucleation, the PCM is partially supercooled (partial blockage) or the PCM is totally supercooled (total blockage). During the nucleation process, the latent heat released by the dendritics ice and consumed by supercooled water, causing the different blockages.
  • 4. photographic image time, s photographic image time, s 0 0 1 1 2 2 2.5 2.5 22.5 6 Figure 3 – The blockage for dendritic ice growth. Acrylic capsule with TC = -16 ºC (left) and TC = -12 ºC (right) The figure 4 represent most of the observed curves (a probability of more than 60%) the blockage for dendritics ice formation, for different capsule materials and different temperatures of the coolant. It can be observed, a zone where the phase change process without the dendritic ice formation, classified as zone of steady processes without supercooling presence. The central area is a blockage’s region, varying according to the material and the coolant temperature. To the right area presents of the metastable liquid region, the liquid remains below of Tm, without a nucleation presence. In the PVC capsule, the majority of the tests did not present supercooling phenomena (without blockage), the process of phase change vary rapidly from steady to metaestable liquid process.
  • 5. Blockage by Dendritic Ice in Supercooled Water Encapsulated Process Bronze SOLIDIFICATION STEADY ZONE (WITH OUT Aluminium SUPERCOOLING) capsule material SOLIDIFICATION METASTABLE ZONE Acrylic LIQUID METASTABLE (WITH SUPERCOOLING) ZONE (WITH PERMANENT SUPERCOOLING) PVC -18 -16 -14 -12 -10 -8 -6 -4 -2 Coolant Temperature, TC, ºC Total blockage Partial blockage to 50% Partial blockage to 25 % Figure 4 – Blockage for dendritic ice for different temperatures of the TF and different materials of the capsule 5. CONCLUSIONS The blockage for dendritic ice growth is a function of the coolant temperature and the capsules material. It can be observed that the presence of total blockage and partial blockage. In the PVC capsule did not present supercooling phenomena (without blockage). For the dendritic ice formation, necessarily the supercooling phenomenon must appear. 6. ACKNOWLEDGEMENTS This paper was supported by the Conselho Nacional de Desenvolvimento Científico e Tecnológico – CNPq of Brazil. The authors also wish to thank the Agreement Pontificia Universidade Católica do Rio de Janeiro and Universidad Católica San Pablo for motivating this research work. NOMENCLATURE TC coolant temperature, [ºC] CTB-IC constant temperature bath of initial PCM phase change material conditions of the PCM CTB constant temperature bath PVC polyvinyl chloride Tm freezing temperature REFERENCES Chen, S. L., Lee, T. Z., 1998, A study of supercooling phenomenon and freezing probability of water inside horizontal cylinders, International Journal of Heat and Mass Transfer 41: (4-5, 3), 769-783. Gilpin, R.R., 1977, The effect of cooling rate on the formation of dendritic ice in a pipe whith no main flow. ASME Journal of Heat Transfer 99: 419-424 Milón, J.J., Braga, S.L., 2003, Supercooling Water in Cylindrical capsules, Fifteenth Symposium on Thermophysical Properties, National Institute of Standards and Technology, Colorado, USA. Milón, J.J., Braga, S.L., 2004, Dendritic Ice Growth in Supercooled Water Inside Cylindrical Capsule, International Refrigeration and Air Conditioning Conference at Purdue, USA. Yoon, J.J., Moon, C.G., E.Kim, Son, Y. S., Kim, J.D., Kato, T, 2001, Experimental study on freezing of water with supercooled region in a horizontal cylinder, Applied Thermal Engineering 21Ç 657-668.