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Qin et al. Miner Miner Mater 2023;2:9
DOI: 10.20517/mmm.2023.20 Minerals and
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Open AccessResearch article
3D montmorillonite aerogel/SA composite phase
change materials with mechanically strong strength
and superior thermal energy storage performances
Lei Qin1, Cong Guo1, Qijing Guo1, Hao Yi1,2 , Feifei Jia1,2
1School of Resources and Environmental Engineering, Wuhan University of Technology, Wuhan 430070, Hubei, China.
2Hubei Key Laboratory of Mineral Resources Processing and Environment, Wuhan University of Technology, Wuhan 430070,
Hubei, China.
Correspondence to: Dr. Hao Yi, School of Resources and Environmental Engineering, Wuhan University of Technology, 122
Luoshi Road, Wuhan 430070, Hubei, China. E-mail: yihao287@whut.edu.cn
How to cite this article: 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. https://dx.doi.
org/10.20517/mmm.2023.20
Received: 20 Jul 2023 First Decision: 21 Aug 2023 Accepted: 20 Sep 2023 Published: 28 Sep 2023
Academic Editors: Yaowen Xing, Lei Xie Copy Editor: Dong-Li Li Production Editor: Dong-Li Li
Keywords: Montmorillonite, stearic acid, phase change materials, aerogel, mechanical strength
INTRODUCTION
With the growth of population, the process of urbanization, and the development of industrialization, the
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.
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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
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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
Mt-based CPCM with excellent mechanical properties, which solves the problem of poor mechanical
strength and takes into account the high heat storage performance. The strong mechanical strength,
excellent thermal storage behavior, and good structure stability of the CPCMs are highlighted in this study.
Having solved the mechanical strength of the aerogel-based CPCMs and improved thermal energy storage
performances, the designed CPCMs show great potential in renewable energy and sustainable development
fields.
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
18.2 MΩ·cm, was used in all experiments.
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,
5 g of SA was uniformly dispersed in the suspension while continuing the stirring for 10 min. The mixtures
were freeze-dried for 12 h, and then the freeze-dried sample was soaked in 49 g of ethanol solution
containing 1 g of CaCl2 for 6 h and subjected to Ca2+ crosslinking to enhance the mechanical strength.
3D-Mt aerogels were obtained after evaporating the alcohol in an oven at 60 °C. Subsequently, a sufficient
amount of SA and 3D-Mt aerogels were placed in a vacuum drying oven at 80 °C for 3 h to make the molten
SA reach adsorption saturation in 3D-Mt aerogels. After vacuum impregnation, the 3D-Mt/SA CPCMs
were placed on filter paper in an atmosphere of 80 °C to remove excess SA.
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
METHODS
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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.
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.
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.
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
Si-O-Al and Si-O-Si[45]. As for sodium alginate, the peak at 3,433 cm-1 is related to the stretching vibration of
the hydroxyl group (-OH). The peaks at 1,620 and 1,421 cm-1 represent the stretching vibration of the
carboxyl group (-COO-); the absorption peak at 1,032 cm-1 corresponds to the stretching vibration of the
alcohol group (-C-OH) (Peng et al., 2017)[45]. In the spectrum of 3D-Mt aerogels, the stretching vibration
of the -COO- group (1,620 cm-1) in sodium alginate and the bending vibration of the H-OH bond
cm-1) in Mt overlap at 1,631 cm-1, which suggests that the hydrogen bond has been formed between
Mt and sodium alginate[46,47].
(1,637
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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.
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
3D-Mt/SA CPCMs had a high degree of crystallinity, the SA was in a crystalline state even after
combination, suggesting good chemical compatibility between the SA and 3D-Mt, and the components
were only combined in a physical form.
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
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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.
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.
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.
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
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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.
Figure 7. Infrared thermography images of pure SA and 3D-Mt/SA CPCMs. CPCMs: Composite phase change materials; Mt:
montmorillonite; SA: stearic acid.
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.
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.
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,
3D-Mt/SA CPCMs increased to 57.4 °C, which was 10.2 °C higher than that of pure SA. This phenomenon
is attributed to the fact that the 3D structure of 3D-Mt aerogels provides a heat transfer path, which
enhances the heat transfer performance and ensures the rapid heat storage of 3D-Mt/SA CPCMs, making it
an ideal choice for efficient thermal energy storage.
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Figure 8. Cycle stability of 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
90 °C heating plate for 40 s and 50 cycles of heating/cooling experiments were performed. Figure 8 shows
the DSC curves of 3D-Mt/SA CPCMs before and after 50 cycles, comparing the data after 50 cycles with the
data before the cycle. The results showed that the melting latent heat of 3D-Mt/SA CPCMs decreased from
183.0 to 165.0 J/g. The slight decrease in latent heat is attributed to the loss of a small amount of molten SA
in the outer layer of 3D-Mt/SA CPCMs, and the decrease in latent heat value is within the appropriate range
of the application. After continuous melting and freezing cycles, 3D-Mt/SA CPCMs can maintain reversible
phase transition without deterioration of phase change performance, so 3D-Mt/SA CPCMs have good cycle
stability and can be reused for heat storage. The relevant results of some clay-based CPCMs are compared.
It can be observed from Table 2 that the loading ratio and latent heat capacity of the 3D-Mt / SA CPCMs in
this study have certain advantages. The Mass ratio and heat storage capacity of the CPCMs have been
improved. In addition, the 3D-Mt/SA CPCMs have good mechanical strength and good application
potential.
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
Table 1. Comparison of the threshold temperature of stability of 3D-Mt/SA CPCMs with other composites
CPCMs Threshold temperature of stability (°C) Ref.
Atapulgite/Capric-Myristic acid eutectic mix composite 156 [57]
Eutectic mixture/Expanded graphite 160 [58]
Ddecylamine/Crbonized clay/pectin aerogels 150 [59]
3D-Mt/SA CPCMs 200 This work
CPCMs: Composite phase change materials; Mt: montmorillonite; SA: stearic acid.
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Table 2. Comparison of latent heat of 3D-Mt/SA CPCMs with previous clay-based CPCMs
CPCMs PCMs mass rate
(%)
Latent heat
(J/g) Ref.
Kaolinite/paraffin 50.9 107.2 [60]
Diatomite/CH3COONa3H2O 63 168.3 [61]
Na-Mt/Paraffinic 31.82 78.78 [62]
OMt/Paraffin 37.1 51.8 [63]
Sepiolite/CaCl2·6H2O 70 87.9 [64]
3D-Mt/SA CPCMs 85.09 183.0 This work
CPCMs: Composite phase change materials; Mt: montmorillonite; PCMs: phase change materials; SA: stearic acid.
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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