Journal Archive

Johnson Matthey Technol. Rev., 2022, 66, (2), 177
doi: 10.1595/205651322X16273773896889

Examination of the Coating Method in Transferring Phase-Changing Materials

Heat regulation in heat storage microencapsulated fabrics

  • Makbule Nur Uyar
  • Akar Tekstil AŞ, İzmir, Turkey
  • Ayşe Merih Sarıışık, Gülşah Ekin Kartal*
  • Dokuz Eylül University, Department of Textile Engineering, Faculty of Engineering, Tınaztepe Campus, İzmir, Turkey
  • *Email: gulsah.kartal@deu.edu.tr

PEER REVIEWED
Received 9th April 2021; Revised 25th May 2021; Accepted 27th July 2021; Online 27th July 2021

Article Synopsis

This study intends to identify the characteristics of heat regulation in heat storage microencapsulated fabrics and to examine the effect of the microcapsules application method. For this purpose, phase-changing material (PCM) microcapsules were applied by impregnation and coating methods on cotton fabrics. The presence and distribution of microcapsules on the fabric surface were investigated by scanning electron microscopy (SEM). The temperature regulation of the fabrics was examined using a temperature measurement sensor and data recorder system (thermal camera). According to the differential scanning calorimetry (DSC) analysis, melting in fabrics coated with microcapsules occurred between 25.83°C–31.04°C and the amount of heat energy stored by the cotton fabric during the melting period was measured as 2.70 J g−1. Changes in fabric surface temperature due to the presence of microcapsules in the fabric structure were determined. When comparing the PCM capsules transfer methods, the contact angle of impregnated and coated fabric was obtained as 42° and 73°, respectively. Analysis of the microcapsules transferred to the fabric by impregnation and coating methods shows that the PCM transferred fabric prepared by the impregnation method performs more efficient temperature regulation. However, the analysis shows that PCM transferred fabrics prepared by coating also perform heat absorption, although not as much as the impregnation method. Performance evaluation according to the target properties of the textile will give the most accurate results for fabrics treated by coating and impregnation methods.

1. Introduction

The importance of functional processes that add value, create difference and increase market share in the textile sector is increasing day by day with developing technology. Not only aesthetic features but also functional features determine consumers’ wishes. For this purpose, technologies like plasma, sol-gel or microencapsulation can provide different functional properties to textile materials (1).

The microencapsulation process produces small spheres covered with a thin shell film to protect the active substance from outside. Using this technology, it is possible to protect easily perishable substances such as drugs, insecticides, antibacterials and antioxidants from environmental factors like heat, light and oxygen. In addition, the wearer is exposed to much lower doses of these substances. Using microcapsules in textile finishing makes it possible to produce resistant-to-wash textile products that are effective even when a less active substance is used. Another area where microcapsules can be used is energy storage (2–6).

Problems like the climate crisis, greenhouse gas emissions, air pollution, usage of finite resources and economic issues require solutions. Energy is needed for heating, air conditioning and ventilation. Energy storage plays an important role in conserving available energy and improving its utilisation since many energy sources, especially renewables, are intermittent. Short-term storage of only a few hours may be desirable in applications like clothes or curtains, while longer-term storage of a few months may be required in some applications like buildings, concrete or space clothes (7–9).

A phase-change material or PCM can store and release large amounts of energy. This energy is called latent heat. Latent heat is thermal energy released or absorbed, by a thermodynamic system, during a constant-temperature process — usually a first-order phase transition. Latent heat can be understood as heat energy in a hidden form which is supplied or extracted to change the state of a substance without changing its temperature. PCMs are classified as latent heat storage units. Each PCM has a specific melting and crystallisation temperature and a specific latent heat storage capacity. PCMs take advantage of latent heat that can be stored or released from material over a narrow temperature range. These materials absorb energy during the heating process as phase change takes place and release energy to the environment in the phase change range during a reverse cooling process. Textiles containing phase change materials react immediately to changes in environmental temperatures and the temperatures in different areas of the body. This system can be used in applications like protective clothing, beds, bedspreads, space suits, diving suits and curtains (10–28).

For any PCM to be used in textile products, it must have certain properties. The main ones are: high melting or hydration temperature, high thermal conductivity, high specific heat capacity, minimum volume change during phase transformation, appropriate phase change temperature, repeatability of phase transformation, low corrosion and degradation tendency and non-toxicity. The textiles should pass certain flame retardancy standards with the PCM material applied. Choosing the appropriate PCM for the protective clothing is crucial for an ideal thermal insulation and regulation effect. Many factors should be taken into consideration while making this choice. What is expected from PCM to be added to a textile product to be used as a garment is to minimise the heat flow between the person and the outside environment by keeping the body temperature constant at a certain value that the person is comfortable with. Suitable materials for textile products in terms of phase change temperatures include: hydrate inorganic salts, polyhydric alcohol-water solution, polyethylene glycol (PEG), polytetramethylene glycol (PTGM), aliphatic polyester, linear long chain hydrocarbons, hydrocarbon alcohols or organic acids (28–39).

In general, the impregnation and exhaustion method can be used to transfer microcapsules in the textile industry. In the impregnation method, a liquor is prepared and the capsules are mixed into this liquor at a certain rate. Afterwards, the fabric is absorbed into the float, passed through a foulard machine and the process is completed with pressure from cylinders. In the coating method, a coating paste is prepared and the capsules are added to the paste at a certain rate. The coating paste is then applied to the fabric. To date, little research has been done on possible applications of microcapsules in functional coating processes.

One of the most important problems of PCMs is low thermal conductivity. For example, paraffin has 0.22 W m−1 K−1 thermal conductivity when compared with >3000 W m−1 K−1 for multiwall carbon nanotubes (MWCNTs). Moreover, microencapsulated PCMs have a polymeric shell, which not only prevents the content from leaking but also resists heat transition. When capsules are transferred to the fabrics by coating, another viscous coating layer is added on the shell material of the capsule. It is thought that this feature will increase in cases where PCM capsules are transferred by the coating method compared to those transferred by the impregnation method (27, 40–42).

Within the scope of this study, it is thought that the coating application can be applied especially in black out curtains. In this study, PCM microcapsules were used to develop thermoregulating textile materials and the effect of the microcapsules application method was examined. In this research, Mikrathermic® P PCM microcapsules were transferred to 100% cotton woven fabrics by the impregnation and coating methods. The thermal regulation properties of the fabrics were analysed by DSC and the surface morphological properties by SEM. In addition, the thermal properties of the fabrics were obtained with a thermal camera. Contact angles and water vapour permeability of coated and impregnated fabrics were investigated.

2. Material and Method

2.1 Material

In this research, desized, 100% cotton fabrics (warp/weft yarn density of 34/17 yarns per centimetre) were used. Mikrathermic® P PCM capsules were provided by Devan Chemicals, Belgium. For the coating process, Mikracat B as a cross linker and L Mikrasoftener as a softener were supplied from Devan Chemicals. RUCO®-COAT PU 1110 polyurethane coating material was used for coating process and supplied from Rudolf Duraner, Turkey. EDOLAN® MR polyurethane binder was used for the impregnation method and provided by Tanatex, Switzerland to bond the microcapsules to the fabric. All other auxiliary chemicals used in the study were of laboratory-reagent grade.

2.2 Application of the Microcapsules to the Cotton Fabrics

The application of the capsules to the cotton fabrics was carried out by impregnation and coating methods. Fabrics were conditioned in accordance with ISO 139:2005 (43) at standard atmospheric conditions (20°C±2 and 65% RH±4) for 24 h. Capsule transfer prescriptions were made according to Tables I and II and in the same ratio to compare the application processes. Polyurethane was selected as binder and each experiment was repeated three times.

Table I

Capsule Transfer Prescription for Impregnation Method

Mikrathermic® P capsule, g l−1 EDOLAN® MR - PUR binder, g l−1 Pick-up ratio, % Drying Fixing
125 30 90 Temperature, °C Time, min Temperature, °C Time, min
80 10 140 3
Table II

Capsule Transfer Prescription for Coating Method

Content Polyurethane paste, g
Mikrathermic® P capsule 125
RUCO®-COAT PU 1110 770
Mikracat B cross-linking agent 100
L Mikrasoftener 5

The capsules were impregnated in a solution bath containing capsules (125 g l−1) and binding agent (30 g l−1), and then squeezed between rollers to 90% wet pick-up. Achieving long lasting effect, the fabric was exposed to drying for 10 min at 80°C and fixation process for 3 min at 140°C in a laboratory stenter (Table I).

Viscosities of the coating pastes were measured using a DV-II+Pro viscometer (AMETEK Brookfield, USA) and the viscosity of the coating paste was determined to be 9000 cps. Cotton base fabrics were coated with the above mentioned coating pastes using a laboratory type blade coating machine, as two layers of coating. It was subjected to intermediate drying at 100°C for 2 min between each layer. Coated samples were cured at 140°C for 3 min.

2.3 Evaluation of Treated Fabrics

SEM images were taken to obtain the existence of capsules on the textile surface from both coated and impregnated samples. Samples were gold-coated (15 mA, 2 min) to assure electrical conductivity. The measurements were taken at 2 kV accelerating voltage. The images were taken at 250× and 1000× magnification.

Thermal properties of the fabrics, such as melting and crystallising temperatures and enthalpies, were measured by DSC performed using a PYRISTM Diamond differential scanning calorimeter (PerkinElmer Inc, USA) to distinguish the capsules on the fabric with the help of characteristic endothermic or exothermic peaks. The samples were cooled down to −20°C and then heated up to 40°C at a constant rate of 10°C min−1 under a nitrogen flow rate of 60 ml min−1.

In order to examine the efficiency of the transferred capsules, the surface temperature of the raw fabric samples containing PCM was measured at a certain time interval by thermal camera as shown in Figure 1. Measurements in the system were made in an insulated box. Before measurement, the inner temperature of the box was heated to a constant temperature of 40°C and the test was carried out at this temperature. The inner temperature of the box was kept constant by means of a thermostat. Before measurement, the fabrics were conditioned for 12 h and placed in the box as quickly as possible. Once the fabric was placed in the box, the surface temperature was measured from a fixed point for 15 min. A thermal camera (Fluke Ti100 Thermal Imager, Fluke, USA; emission value 0.94) was used in the measurements and the temperature was recorded every 30 s.

Fig. 1.

Thermal camera system (18)

When an interface exists between a liquid and a solid, the angle between the surface of the liquid and the outline of the contact surface is described as the contact angle θ (lower case theta). The contact angle (wetting angle) is a measure of the wettability of a solid by a liquid. In order to examine the hydrophilicity of the fabrics, the contact angle was examined. The measurements were carried out at 25°C using the Theta Lite T101 (Biolin Scientific, Sweden) model contact angle device. An image of approximately 5 μl of water droplet dropped onto the surface to be measured was recorded for 10 s by the device camera. Using the device software, an average of 200 data were recorded for 10 s for each sample and the arithmetic mean was taken.

Water vapour permeability is related to breathability of fabrics. Water vapour permeability of samples was determined by using M261 (SDL Atlas International, USA) model water vapour permeability tester according to BS 3424-34:1992-Method 37 (44). The amount of water vapour passed through the samples was determined after 24 h and permeability values were calculated. The test was repeated three times for each sample type.

3. Results and Discussion

After the capsules containing PCM were transferred to cotton fabrics by impregnation and coating methods, analyses were carried out on the fabrics.

3.1 Scanning Electron Microscopy

SEM images of the Mikrathermic® P PCM capsule are shown in Figure 2. Mikrathermic® P was around 3 μm and had a spherical shape as expected. SEM images of the PCM capsules transferred to cotton fabrics by coating and impregnation methods, enlarged 250 times and 1000 times, are given in Table III.

Fig. 2.

SEM images of Mikrathermic® P capsules (1000×)

Table III

SEM Photomicrographs of Fabrics Treated with PCM Capsules

Fabric 250× 1000×
Coated
Impregnated

When the images were examined morphologically, it was observed that the capsules transferred by the impregnation method preserved their spherical form. PCMs transferred by coating remain under the coating polymer and were homogeneously distributed over the entire surface. These images showed that capsule application was successful for both impregnation and coating methods. It was observed that capsules were covered with the binder and fixed onto the textile surface of the cotton fabrics.

3.2 Differential Scanning Calorimetry Analysis

The DSC diagrams of coated and impregnated fabrics are given in Figure 3. The heat storage capacity of the Mikrathermic® P PCM microcapsule is 140 J g−1 according to the literature (45–47). From the DSC curve given in Figure 3 and from Table IV, the amount of heat stored and emitted by the fabrics from the area under the endothermic and exothermic melting and solidification peaks and the temperatures at which heat storage and emission begins can be seen. According to the DSC analysis, similar values were obtained for coated and impregnated fabrics. The values are provided in Table IV in detail.

Fig. 3.

DSC diagrams of coated and impregnated fabrics with PCM capsules

Table IV

Thermal Properties of Coated and Impregnated Fabrics

Fabric Melting point, °C Melting enthalpy, J g−1 Crystallisation point, °C Crystallisation enthalpy, J g−1
Coated 25.83 2.70 25.70 −1.45
Impregnated 25.72 2.64 25.61 −1.39

The melting process in fabrics coated with Mikrathermic® P microcapsules occurred between 25.83°C–31.04°C and the amount of heat energy stored by the cotton fabric during the melting period was measured as 2.70 J g−1. For the Mikrathermic® P microcapsule, the crystallisation process occurred in the range of 25.70°C–23.45°C and the cotton fabric released −1.45 J g−1 heat during crystallisation. Impregnated fabric absorbed 2.70 J g−1 at 25.72°C during melting and released −1.39 J g−1 at 25.61°C during crystallisation.

Thermal conductivity measures the capacity of temperature exchange between heat and cold passing through a material mass. Decreased thermal conductivity allows for a faster rate of heat transfer in a PCM, increasing the time required for the PCM to undergo a complete charge or discharge. The major shortcoming of PCM is its limited ability to exchange heat effectively due to low thermal conductivity. This suppresses the amount of heat that can be exchanged during melting processes and a lower thermal conductivity of solidification will occur at low temperatures. The effective thermal conductivity of PCM can be increased by many mechanisms such as inserting fins and adding a dispersion of high thermal conductivity nanoparticles (48, 49).

Although the process temperatures are very close to each other, coated fabrics changed state at higher temperatures compared to impregnated fabrics. The shifting of the process peaks to higher temperatures has been explained in the literature as the lower thermal conductivity of the fabric (50). This situation was interpreted as the lower thermal conductivity value of coated fabrics compared to impregnated fabrics resulting in melting and solidification at higher temperatures. However, considering that these data are very close to each other, it was thought that the capsules can be transferred to the fabrics by the coating method. Encapsulated PCMs which were transferred with coating and impregnation lead to lower thermal conductivity and increased heat capacity of a textile structure. They improve the thermal performance of textile material and therefore may save energy.

3.3 Thermal Camera

Depending on the change in ambient temperature, the fabric surface temperature change caused by PCM capsules was measured. For this purpose, a thermal camera was used to determine the heat regulation properties of fabrics that can store heat. Two measurements were taken from two different points in the fabric samples and their averages are shown in Figure 4.

Fig. 4.

Thermal camera results of the fabric

The temperature-time curves are given in Figure 4. It can be seen from the graphs that the fabrics which were brought from a cold environment (4°C±2) to a warm environment (40°C±2) were warmed and the temperatures measured on their surfaces increased. On the other hand, it is observed that the heating time of the fabrics in a hot environment and the maximum temperatures reached were not equal. According to both measurement results, it can be seen that the raw fabric heats up the fastest. Similarly, the maximum surface temperature of the raw fabric was higher than the fabrics containing PCM. The raw fabric warmed to almost maximum temperature (about 42°C) in about 5 min. For fabrics containing PCM, the maximum temperature recorded was lower at the end of the measurement period. The maximum value recorded was 37°C for the fabric in which the PCM capsules were impregnated and 40–41°C for the fabric transferred with the coating. Thermal camera analysis was performed for 15 min. It was determined that the temperature of the fabrics remained at the last point which they reached for an extended period. During the measurement period, it was determined that the temperature measured on the surface of the fabric to which the PCM capsules were impregnated was 3°C to 5°C lower than the raw fabric surface temperature. It was determined that the surface temperature of the fabric to which the PCM capsules were transferred with the coating was 1–3.5°C lower than the raw fabric.

When the analysis results were evaluated, it was seen that the fabric with PCM transferred by the impregnation method has more effective temperature regulation. The impregnated fabric, which has the lowest temperature, absorbed more heat in the cold environment when the PCM structure was applied. It also appears that there was not a big difference between coating and impregnation methods in thermal camera analysis. The thermal camera method demonstrates the heat regulation ability of fabrics, but does not provide information about their performance in end-use areas. Therefore, for fabrics treated with coating and impregnation methods, performance evaluation according to the area of use will give the most accurate results. This shows that PCM capsules can also be transferred by the coating method, depending on the usage areas.

3.4 Contact Angle Measurement

In order to evaluate the hydrophilicity properties of raw fabric and PCM-transferred fabrics with different methods, contact angle measurement was made as shown in Figure 5.

Fig. 5.

Contact angle images of fabrics: (a) raw fabric; (b) coated fabric; (c) impregnated fabric

The angle between the surface of the liquid and the outline of the contact surface is described as the contact angle θ. The contact angle is a measure of the wettability of a solid by a liquid. In the case of complete wetting, the contact angle is 0°. Between 0° and 90°, the solid is wettable and above 90° it is not wettable. When the analysis results were examined, water was completely absorbed by raw fabric in 5 s and this indicates that the fabric is hydrophilic. When comparing the transfer methods of PCM capsules, contact angle of impregnated and coated fabric was obtained as 42° and 73°, respectively. In general, the coating paste has a more viscous structure and this structure causes a thick layer to form on the fabric. Due to this structure, the surface energy of the fabric decreases and it gains water repellency. In the impregnation method, since a viscous structure is not obtained and a layer is not formed on the fabric surface, the contact angle becomes lower causing the textile material to be more hydrophilic than the coated one. This result, as expected, was that the coated fabric was more hydrophobic than the impregnated fabric.

3.5 Water Vapour Permeability

Water vapour permeability analysis was carried out to examine the comfort properties of the fabrics obtained. Water vapour permeability of samples are tabulated in Table V.

Table V

Water Vapour Permeability Results of Fabrics

Fabric Water vapour permeability, g m−2 per 24 h
Raw 625.44
Impregnated 619.02
Coated 352.18

The highest water vapour permeability was obtained from raw fabric with 625 g m−2 per 24 h permeability value. It was determined that the fabrics with PCM transferred by the impregnation method gave a similar result to the raw fabric. On the other hand, water vapour permeability of coated samples reduced to approximately 50% that of the raw base fabric in parallel with the contact angle results. This was due to the additional polyurethane coating layer which contributed mass transfer limitation through the fabric. Even the most breathable coating polymer applied to the samples would add a resistance to vapour flow by closing the pores and creating an additional layer (51). The water vapour permeability of a material plays an important part in evaluating the physiological wearing comfort of clothing systems or determining the performance characteristics of textile materials used in technical applications. Therefore, it is important to choose the transfer method of PCM capsules considering the area where the fabric will be used.

4. Conclusion

Within the scope of this study, PCM capsules were applied to textile materials with coating and impregnation methods, successfully. As a result of the study, it was observed that the capsules transferred by the impregnation method preserved their spherical form according to the SEM images. It was seen that PCMs transferred by coating remain under the coating polymer and were homogeneously distributed over the entire surface. When thermal properties of coated and impregnated fabrics were examined with DSC analyses, it was seen that thermal behaviours of fabrics treated by the impregnation and coating methods were similar.

According to the results of the thermal camera analysis, it was seen that the PCM transferred fabric with the impregnation method performs more effective temperature regulation than the coating method. The fabric with PCM transferred by the impregnation method makes more effective temperature regulation. The impregnated fabric, which has the lowest temperature, absorbed more heat in the cold environment when the PCM structure was applied. The impregnation method showed slightly better results according to the thermal camera although it was close to the coating method. As predicted, the contact angle of the coated fabric was higher and the air permeability was lower than the impregnated fabric. However, the thermal results obtained show that PCM capsules can also be transferred by the coating method. This situation makes the end use area of the fabric to be used important.

There are lots of clothing comfort properties of textiles such as heat transfer, thermal protection, air permeability, moisture permeability and water repellence. While it may be preferred to use the impregnation method where comfort features are important, PCM capsules can be transferred by the coating method if comfort features are not important. Performance evaluation according to the target properties of textile material will give the most accurate results for fabrics treated by coating and impregnation methods. The coating method may be an alternative to the impregnation method. Based on these results, fabrics in which the capsules are transferred by coating can be used in black out curtains. Fabrics to which capsules are transferred by impregnation can be used in bedding fabrics or clothes considering their comfort properties.

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Acknowledgements

We especially thank Associate Professor Sennur Alay Aksoy from Süleyman Demirel University, Turkey, for thermal camera analysis.

The Authors

Makbule Nur Uyar is a textile engineer. She graduated from Dokuz Eylül University, Turkey, in 2017. Currently she is working at Sun Textile as collection fabric buyer in the research and development department.

Merih Sariişik is a Professor in the Textile Engineering Department, Dokuz Eylül University, Ýzmir, Turkey. She has 34 years’ teaching and research experience. Her research interests are micro/nano encapsulation technology, enzyme treatment in textiles, medical textiles and layer-by-layer technology in textile treatment.

Gülşah Ekin Kartal is currently working as a Research Assistant in the Textile Engineering Department, Faculty of Engineering, Dokuz Eylül University, Ýzmir, Turkey. She received her master’s and PhD degrees from the Textile Engineering Department, Dokuz Eylül University. Her research interests are micro/nano encapsulation technology, functional textile finishing, textile dying, textile printing, layer-by-layer technology in textile treatment, liposomes and fishing nets.

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