3D montmorillonite aerogel/SA composite phase change materials with mechanically strong strength and superior thermal energy storage performances
0 Abstract
Phase change materials (PCMs) often suffers leakage when used in thermal energy storage. In this work, for the sake of preventing leakage, three-dimensional interconnected montmorillonite aerogel (3D-Mt) has been designed through self-assembly method to encapsulate stearic acid (SA) as composite PCMs. The as prepared 3D-Mt with porous structure has encapsulated large amount of SA, which resulted in a high phase change enthalpy of 183 J/g. In addition, due to the surface tension and capillary forces of 3D-Mt aerogels, the SA were confined in the pore structure tightly, leading to excellent structural stability and good cycling performances during continuous solid-to-liquid phase change. In addition, due to the protection of 3D-Mt, the composite PCMs showed good shape stability and high mechanical strength. The prepared 3D-Mt/SA CPCMs can withstand a weight of 500 g without any deformation, and the loads are as high as 1.01 and 13.81 MPa under 55% and 80% deformation, respectively. With high heat storage capacity, good thermal stability, and excellent mechanical strength, the prepared 3D-Mt/SA CPCMs shows great application potential in the field of thermal energy storage.
Keywords
INTRODUCTION
With the growth of population, the process of urbanization, and the development of industrialization, the consumption and demand for energy have surged dramatically[1-3]. Non-renewable energy sources, such as fossil fuels, have been overexploited, causing global warming and other serious environmental pollution[4,5]. In order to cope with the challenges from resource depletion and environmental contamination and solve the problem of mismatch between energy supply and demand, the utilization of sustainable energy is an important initiative[6-8]. Solar thermal energy has drawn considerable attention due to the characteristics of large reserves and no contamination, which can be used as an ideal alternative energy source[9,10]. The development and utilization of solar thermal energy is one of the most effective ways to deal with the shortage and depletion of traditional energy. Considering the intermittency, randomicity, and low energy density, which affect the utilization efficiency of solar thermal energy, it is of great significance to develop reliable, cost-effective solar energy collection and energy storage technologies[11,12]. Phase change materials (PCMs) can store/release heat by undergoing phase change in a small temperature range, which helps to improve energy utilization efficiency and is one of the ideal solutions to energy shortages and environmental problems[13,14]. Organic PCMs, such as stearic acid (SA), paraffin, polyethylene glycol (PEG), etc., with the advantages of high energy storage density, good chemical stability, and non-toxicity, have been widely studied and applied in thermal management fields such as building materials[15,16], solar energy storage[17-19], electronic equipment cooling[20,21], and industrial waste heat recovery[22,23] in recent years. SA is a kind of fatty acid widely existing in nature. It is widely used in PCMs[24,25], surfactants[26,27], pharmaceuticals[28,29], etc. It is considered to be a material with appropriate phase transition temperature and good latent heat capacity[30,31]. However, organic PCMs suffer from some challenges in the application, such as melting leakage, poor shape stability, and bad mechanical stability, which seriously limits the large-scale application of PCMs in the field of thermal management[32,33].
In order to solve the leakage problem of PCMs, some techniques have been developed, including microencapsulation[34,35] and shape stability technology. For example, Mohaddes et al. successfully used melamine-formaldehyde resin as the shell material to encapsulate n-eicosane, and the latent heat of melting of the microcapsules exceeded 162.4 J/g, which has good leakage resistance[36]. Li et al. encapsulated PEG in zirconium phosphate/polyvinyl alcohol composite aerogel by vacuum impregnation method, and the prepared composite PCMs (CPCMs) could maintain their shape stability during the PEG phase transition process[37]. Yang et al. combined self-assembly and chemical vapor deposition (CVD) technology to encapsulate hybrid graphene aerogel in graphene foam for encapsulation of paraffin[38], and the resulting CPCMs have good shape stability and high heat storage density[39]. Recently, it has been proved that CPCMs, supported by aerogels with high porosity, large specific surface area, and huge adsorption capacity, often show larger latent heat capacity while preventing leakage. However, most of the aerogel-based CPCMs have poor mechanical strength, which is liable to break under external force and lead to the risk of leakage. Therefore, exploring a simple and efficient method to prepare CPCMs with high heat storage performance and excellent mechanical properties is still a hot topic in the field of thermal management[40,41].
In this study, a mechanically strong aerogel has been designed to prepare CPCMs in order to improve shape stability. Montmorillonite (Mt) is a natural clay mineral with a layered structure that can be effortlessly exfoliated into 2D nanosheets. Besides, the Mt nanosheets can be easily assembled into aerogel under the action of a crosslinking agent. In previous literature, it turned out that the addition of Mt in the organic aerogel can greatly promote the mechanical strength (Biswas et al., 2019)[42]. At the same time, sodium alginate is a general crosslinking agent that can be used to synthesize organic aerogel. As a consequence, the mechanically strong aerogel is designed through a self-assembled method by using Mt integrated with sodium alginate; the obtained aerogel with abundant pores can encapsulate a large amount of PCMs and lead to large latent heat capacity. Besides, the addition of Mt can reinforce the mechanical strength of the Mt aerogel and the CPCMs, which will benefit the shape stability and cycling performances of the CPCMs[24]. In addition, the obtained CPCMs can effectively prevent leakages during solid-to-liquid phase change owing to surface tension and capillary forces of the 3D-Mt aerogel. The innovation of this study is to prepare a
METHODS
Materials
SA, sodium alginate, calcium chloride (CaCl2), and absolute ethanol (C2H6O, 99.7%) were purchased from Shanghai Sinopharm Chemical Reagent Co., Ltd. All chemicals were used without further purification. Mt was acquired from Chifeng Ningcheng Montmorillonite Company Limited (Inner Mongolia, China). Deionized water, produced by a Milli-Q ultra-pure water meter (Milli-Q, US) with a resistivity of
Preparation of 3D-Mt/SA CPCMs
3D-Mt/SA CPCMs are prepared by vacuum impregnation, and the specific preparation steps are as follows: First, 5 g of Mt was added to 100 mL of deionized water and was stirred for 10 min at 25 °C. Subsequently,
Characterization
Fourier transform infrared spectroscopy (FTIR, Nicolet 6700) was used to analyze the chemical structure of samples and the compatibility between components in the wavelength range of 400-4,000 cm-1. The X-ray diffraction patterns of the samples were obtained by X-ray diffractometer (XRD, Bruker, Germany). The morphology and structure of the samples before and after vacuum impregnation were characterized by scanning electron microscopy (SEM, Phenom ProX) at an accelerating voltage of 15 kV. A differential scanning calorimeter (DSC, Discovery DSC25 - TA Instruments) was used to investigate the thermal properties of the samples at a heating/cooling rate of 2 °C/min under a nitrogen atmosphere. Thermogravimetric (TG) analysis of samples is performed via a thermal analyzer (NETZSCH STA 449 F5) from room temperature to 600 °C to investigate the thermal stability of the sample. An infrared camera (FOTRIC 224s) was used to record the temperature change of the sample during the heat storage process, and in this test, a xenon lamp was used to simulate sunlight to provide a heat source. Microcomputer-controlled electro-hydraulic servo universal testing machine (SHT4106) is used to study the mechanical strength of samples.
RESULTS AND DISCUSSION
Structural morphology of 3D-Mt/SA CPCMs
The morphology of 3D-Mt/SA CPCMs was studied by SEM. As shown in Figure 1A, it can be observed that the 3D-Mt aerogels have interconnected sheet-like porous structures, providing a large amount of adsorption space for the molten PCMs, which is responsible for better thermal storage properties per unit volume. As shown in Figure 1B, in the structure of 3D-Mt/SA CPCMs, SA is embedded and uniformly dispersed in the porous network structure of 3D-Mt aerogels. The porous structure of 3D-Mt aerogels provides surface tension and capillary forces to confine molten SA in the pore structure with the purpose of preventing leakage.
Figure 1. SEM images of (A) 3D-Mt aerogels and (B) 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid; SEM: scanning electron microscopy.
Synthesis mechanism of 3D-Mt/SA PCMs
The interaction of each component affects the latent heat storage performance of 3D-Mt/SA CPCMs, so the synthesis mechanism of 3D-Mt/SA CPCMs has been studied by FTIR. Figure 2A shows the FTIR spectra of Mt, sodium alginate, and 3D-Mt aerogels. In the spectrum of Mt, the broad absorption band at 3,442 cm-1 corresponds to the O-H stretching vibration[43]; the recorded peak at 1,637 cm-1 is attributed to the bending vibration of the H-OH bond[44] (Brahmi et al., 2021). The peak at 1,034 cm-1 is caused by the stretching vibration of Si-O; the absorption peaks at 521 and 466 cm-1 are usually related to the bending vibration of
Figure 2. (A) FTIR spectra of Mt, sodium alginate, and 3D-Mt aerogels; (B) FTIR spectra of SA, 3D-Mt, and 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; FTIR: fourier transform infrared spectroscopy; Mt: montmorillonite; SA: stearic acid.
The chemical compatibility of SA and 3D-Mt aerogels was further studied. Figure 2B shows the FTIR spectra of 3D-Mt/SA CPCMs, SA, and 3D-Mt aerogels. In the pure SA spectrum, the absorption peaks at wavenumbers 2,918 and 2,849 cm-1 correspond to the symmetric stretching vibrations of -CH3 and -CH2, respectively. The strong absorption peak at 1,704 cm-1 represents the stretching vibration of C=O[45,48,49]. The peaks at 1,468 and 1,297 cm-1 are the absorption peaks of the in-plane bending vibration of -OH functional group; the peaks at 944 and 722 cm-1 are attributed to the out-of-plane bending vibration and in-plane rocking vibration of -OH functional group, respectively[50-53]. In the spectra of 3D-Mt/SA CPCMs, all absorption peaks correspond to SA and 3D-Mt aerogels, and no new peaks are generated. This result indicated that no chemical reaction occurred between SA and 3D-Mt aerogels. The molten SA is adsorbed in the pores of the 3D-Mt aerogels through capillary and surface tension.
Chemical compatibility of 3D-Mt/SA CPCMs
By comparing the XRD patterns of 3D-Mt/SA CPCMs with Mt and SA, it is further judged and analyzed whether the components in CPCMs undergo chemical reactions to produce new substances. Figure 3 shows the XRD spectra of SA, Mt, and 3D-Mt/SA CPCMs. It can be seen from the figure that pure SA has two strong diffraction peaks at 2θ = 21.8° and 2θ = 24.3° and a weak diffraction peak at 2θ = 11.4°. In the XRD spectra of 3D-Mt/SA CPCMs, the diffraction peaks are mainly caused by the crystallization of SA components, and the peaks observed at 2θ = 21.8° and 2θ = 24.3° overlap with the characteristic peaks of SA. However, the peak intensity at 2θ = 21.8° decreased, which was mainly attributed to the smaller crystallite size of SA in CPCMs due to the confinement of aerogel pore structure[54,55]. XRD results showed that the
Figure 3. XRD spectra of SA, Mt, and 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid; XRD: X-ray diffractometer.
Mechanical strength of 3D-Mt/SA CPCMs
High mechanical strength is one of the necessary conditions for 3D-Mt/SA CPCMs to maintain structural stability in practical applications, so this experiment explored the mechanical stability of the material. Mt, as a supporting frame, can enhance the stability of the structure[56]. As shown in Figure 4A, the 3D-Mt/SA CPCMs did not undergo obvious deformation after placing the weights of 100 and 500 g on the upper surface of 3D-Mt/SA CPCMs, and no cracks were observed. Stress-strain tests were further carried out, and the results are shown in Figure 4B. The stress-strain curves of 3D-Mt/SA CPCMs can be divided into three parts: at low strains of < 5% corresponding to rigid elastic deformation; the strain between 5% and 55% is the plastic deformation platform; high strains of > 55% lead to an exponential increase in stress per strain due to plastic deformation and densification, implying the loss of the characteristic 3D interconnected network structure of 3D-Mt/SA CPCMs. The results showed that the 3D-Mt/SA CPCMs exhibited excellent mechanical strength with loads of 1.01 MPa at 55% strain and 13.81 MPa at 80% strain.
Figure 4. (A) 3D-Mt/SA CPCMs under different weight loads; (B) Compressive stress-strain curve of 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid.
Thermal stability and shape stability of 3D-Mt/SA CPCMs
Thermal stability is an important factor for the practical application of 3D-Mt/SA CPCMs, and the thermal degradation temperature of 3D-Mt/SA CPCMs and their components were determined by TG analysis. Figure 5 shows the TG curves of pure SA, Mt, and 3D-Mt/SA CPCMs. The results showed that there was a one-step thermal decomposition process of SA in the range of 200-320 °C, and the slight weight loss of Mt below 100 °C was attributed to the evaporation of adsorbed water. In the TG curves of 3D-Mt/SA CPCMs, a decomposition trend was shown to be similar to that of pure SA. At temperatures below 320 °C, most of the weight loss was attributed to the removal of SA in the composites, and the weight loss at temperatures above 320 °C was mainly due to the degradation of the main chain of SA in aerogels. In addition, the onset temperature of weight loss of 3D-Mt/SA CPCMs is lower than that of pure SA, which is mainly attributed to the thermal conduction path provided by the aerogel framework, which accelerates the decomposition of SA. The comparison of the threshold temperature of stability in our work and other composites is listed in Table 1. It can be observed that the 3D-Mt/SA CPCMs have good thermal stability.
Figure 5. TG curves of pure SA, 3D-Mt, and 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid; TG: thermogravimetric.
Comparison of the threshold temperature of stability of 3D-Mt/SA CPCMs with other composites
In order to explore the shape stability of 3D-Mt/SA CPCMs, the anti-leakage test was carried out. Figure 6 shows the shape pictures of pure SA and 3D-Mt/SA CPCMs heated on a 90 °C heating plate for various durations. It can be seen from the photo that pure SA melts quickly during the heating process and basically melts into a liquid after heating for 40 s. After heating, the surface of 3D-Mt/SA CPCMs was wetted, but almost no liquid leaked out on the filter paper. 3D-Mt aerogels provide a strong 3D framework structure for SA, which can confine the molten SA in the pore structure, which is beneficial to preventing leakage. The results show that the 3D-Mt/SA CPCMs have excellent shape stability and can maintain their shape even at high temperatures.
Figure 6. Shape pictures of pure SA and 3D-Mt/SA CPCMs heated for varying durations. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid.
Thermal energy storage properties of 3D-Mt/SA CPCMs
The temperature response speed determines the heat storage/release efficiency of PCMs. In this experiment, a heat source is provided above the sample by xenon lamp light, and the thermal response of the sample is evaluated by monitoring the temperature change of the sample by an infrared camera. The results are shown in Figure 7; the temperature of pure SA increased from room temperature to 29.7 °C after 30 s of light irradiation, while that of 3D-Mt/SA CPCMs increased to 36.2 °C. After 120 s of light irradiation,
Figure 7. Infrared thermography images of pure SA and 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid.
Phase change performance and cycle stability are the key parameters affecting the practical application of 3D-Mt/SA CPCMs. CPCMs continuously undergo phase transitions under heat storage and release conditions, and the storage state of SA in 3D-Mt aerogels is also changing, which will have a certain impact on the heat storage and heat release properties of the materials. The 3D-Mt/SA CPCMs were heated on a
Figure 8. Cycle stability of 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid.
Comparison of latent heat of 3D-Mt/SA CPCMs with previous clay-based CPCMs
In conclusion, a method for preparing 3D-Mt/SA CPCMs with excellent mechanical strength and heat storage is provided. In these CPCMs, 3D-Mt aerogels were used as a support material to encapsulate SA, which effectively solved the main problem of easy leakage of PCMs. The melting enthalpy of 3D-Mt/SA CPCMs is as high as 183 J/g, and it can be kept stable for 50 melting/freezing cycles, showing an excellent heat storage effect. In addition, the prepared 3D-Mt/SA CPCMs can withstand a weight of 500 g without any deformation, and the loads are as high as 1.01 and 13.81 MPa under 55% and 80% deformation, respectively, showing excellent mechanical properties. Based on the high heat storage capacity, excellent mechanical strength, and thermal stability of 3D-Mt/SA CPCMs, these CPCMs possess great potential for applications in thermal energy management and conversion systems in complex environments.
DECLARATIONS
Authors’ contributions
Conceptualization, methodology, investigation, writing, review and editing: Qin L, Guo C
Methodology, investigation: Guo Q
Conceptualization, review and editing, technical, and material support: Yi H, Jia F
Availability of data and materials
Not applicable.
Financial support and sponsorship
This work was supported by the National Natural Science Foundation of China (52104265).
Conflicts of interest
All authors declared that there are no conflicts of interest.
Ethical approval and consent to participate
Not applicable.
Consent for publication
Not applicable.
Copyright
© The Author(s) 2023.
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Qin, L.; Guo C.; Guo Q.; Yi H.; Jia F. 3D montmorillonite aerogel/SA composite phase change materials with mechanically strong strength and superior thermal energy storage performances. Miner. Miner. Mater. 2023, 2, 9. http://dx.doi.org/10.20517/mmm.2023.20
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