Accepted Manuscript

Fabrication and characterization of fatty acid/wood-flour composites

as novel form-stable phase change materials for thermal energy
storage

Jiang Liang , Liu Zhimeng , Yuan Ye , Wang Yanjun , Lei Jingxin ,

Zhou Changlin

PII: S0378-7788(18)30843-0
DOI: 10.1016/j.enbuild.2018.04.044
Reference: ENB 8517

To appear in: Energy & Buildings

Received date: 14 March 2018

Revised date: 17 April 2018
Accepted date: 22 April 2018

Please cite this article as: Jiang Liang , Liu Zhimeng , Yuan Ye , Wang Yanjun , Lei Jingxin ,
Zhou Changlin , Fabrication and characterization of fatty acid/wood-flour composites as novel form-
stable phase change materials for thermal energy storage , Energy & Buildings (2018), doi:
10.1016/j.enbuild.2018.04.044

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 ACCEPTED MANUSCRIPT

Fabrication and characterization of fatty acid/wood-flour

composites as novel form-stable phase change materials for
thermal energy storage
Jiang Liang, Liu Zhimeng, Yuan Ye, Wang Yanjun, Lei Jingxin*, Zhou Changlin*
State Key Laboratory of Polymer Materials Engineering, Polymer Research Institute
of Sichuan University, Chengdu 610065, China

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*Corresponding authors.

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E-mail addresses: jxlei@scu.edu.cn (J. Lei); chouscu@scu.edu.cn (C. Zhou).

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Abstract

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The fatty acid (FA)/wood-flour (WF) composite form-stable phase change
materials (PCMs) were prepared via a direct impregnation method, in which WF was
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selected as the supporting materials. The surface morphology, chemical structure,
crystalline structure, phase change properties, thermal reliability and stability of the
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prepared FA/WF composite form-stable PCMs were investigated by scanning electron

microscopy (SEM), Fourier transform infrared spectrometer (FTIR), X-ray diffraction
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(XRD), differential scanning calorimeter (DSC), accelerated thermal cycling testing

and thermogravimetric analysis (TG), respectively. SEM images showed that the
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porous spaces of WF can be largely occupied by the impregnated FA without leakage.

FTIR and XRD results suggested that there was no chemical reaction but only
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physical interactions between WF and FA. XRD analysis also demonstrated that the
WF had no effect on the crystallization of FA. The prepared FA/WF composite PCMs
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had high latent heats and a suitable phase change temperature range, especially the
maximum latent heats in melting and freezing process for the HW-FSPCM reached
102.6 J/g and 103.5 J/g. The prepared FA/WF composite PCMs exhibited
comprehensive thermal reliability and stability from the thermal cycling test and TG
analysis.
Keyword: Form-stable phase change material; Wood-flour; Fatty acids; Thermal
properties.
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1. Introduction
Efficient energy storage devices and systems are essential for protecting the
environment due to the continuous increase in greenhouse gas emissions and the
depletion of fossil fuels [1-4]. In order to address the energy crisis, the increasing
consideration of thermal energy storage (TES) has been paid to phase change materials
(PCMs) because they have high-energy storage density to absorb and release
abundant heat during the heat storage and release process at their phase transition

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temperature (PTT) [5-7]. Therefore, PCMs have been broadly applied in the field of

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solar energy utilization, buildings materials, waste heat recovery, central

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air-conditioning systems and smart fibers [8-12]. In the last decades, various pristine
organic PCMs including paraffin waxes [8,13,14], fatty acids [2, 11, 15], fatty alcohol

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[16, 17] and polyethylene glycol (PEG) [4, 12, 18] have been studied and applied
extensively for thermal energy storage (TES) due to their advantages of high latent
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heats, numerous species and cheapness. However, the PCMs will be turned into fluid
state above the corresponding PTT. To solve the problem of the PCMs leaking-out
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once melted, the effective capsulation of PCMs can be employed by using

microencapsulated PCMs with incorporating PCMs into a thin polymeric shell [19]
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and granular PCMs composites with incorporating PCMs into different types of
porous supporting materials [20]. Compared with microencapsulated PCMs, granular
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PCM composites are great economical, stable, and sustainable, which has become a
research hotspot [21-24].
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Recently, several reports that different kinds of form-stable PCMs have been
prepared by using an inorganic material with a porous/lamellar structure or a polymer
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with a high melting point as containers [25-27]. In order to enhance the effective
capsulation, many porous/lamellar materials, such as diatomite [28, 29], vermiculite
[11, 30], carbon nanofillers [31] and nanotubes [32], expanded graphite [8, 33] and so
on, have been used to prepare organic and inorganic composite form-stable PCMs.
Sarı etc al. [28] reported that the prepared diatomite/carbon nanotubes/polyethylene
glycol composite PCMs exhibited no leakage with the maximum value of 51.7%
polyethylene glycol and different carbon nanotubes contents. Karaipekli et al. [30]
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prepared capric-myristic acid/vermiculite composite form-stable phase change

material and concluded that the capric-myristic acid eutectic mixture could be
retained by 20 wt% into pores of the vermiculite without melted PCM seepage. As for
organic phase change materials, fatty acids and and their eutectic mixtures are the
promising candidates to prepare the organic composite form-stable PCMs due to their
advantages of the high phase change enthalpy, good thermal and chemical stability,
low cost, non-toxicity, and wide range of melting temperatures [34-36]. The merit of

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form-stable PCMs is that PCMs can avoid the liquid leakage and corrosion behavior

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of energy storage units while the ambient temperature is higher than the phase change

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temperature. Li et al. [37] investigated the binary fatty acid/diatomite composites as
form-stable PCMs based on the eutectic caprice-lauric acid blends. The latent heat of

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binary acid/diatomite composite reached 66.81 J/g when 57 wt% of caprice-lauric
acid blends was absorbed into the porous diatomite. Han et al. [38] revealed the
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sebacic acid and mesoporous MCM-41composite shape-stabilized phase change
material by a facile blending and impregnating method. It included that the PCMs
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composite with 70 mass% SA is the most promising candidate for heat storage
application. Zhang et al. [39] reported that the thermal conductivity of stearic acid (SA)
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and modified expanded vermiculite (EV) shape-stabilized composite phase change

materials can be apparently enhanced when 63.12 wt % of SA was retained in the
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SA/EVC ss-CPCMs without leakage.

It was mentioned above, porous materials selected as the support matrixto prepare
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the form-stable PCMs, can be found in many scientific literatures. WF are low density,
high porosity, high absorption capability, inertness and cheapness [40, 41], which is a
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good candidates as supporting materials for applications in buildings. The structure of

WF is made of cellulose fibers in an amorphous matrix of lignin, hemicellulose and
cellulose, containing a large number of hydroxyl groups [42]. Therefore, organic
PCMs can be incorporated into WF by hydrogen-bond interaction, capillary force and
surface tension force to prevent the leakage during the phase transition process [43].
However, few previous studies reported that WF was selected as supporting materials
to encapsulate organic PCMs for the preparation for form-stable PCMs [44-46].
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Additionally, WF can be used to prepare various wood-based boards as a structural

material for building and furniture construction. Thus, the prepared FA/WF composite
form-stable PCMs have potential application in wallboard insulation materials for
thermal energy storage because of the superior thermal properties and easy synthesis
[44, 45].
In this study, the fatty acid (lauric acid, myristic acid, hexadecanoic acid and stearic
acid) and WF composite were prepared by a direct impregnation method. The

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chemical composition, crystalline properties, phase change properties, thermal energy

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storage mechanism, and thermal stability of FA/WF form-stable PCMs were

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investigated via Fourier transform infrared spectroscopy, X-ray diffraction,
differential scanning calorimetry, polarizing optical microscopy and

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thermogravimetric analysis, respectively. An accelerated thermal cycling testing was
also performed to reveal the thermal reliability of FA/WF form-stable PCMs.
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2. Experimental
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2.1. Materials
The fatty acids (FA) including lauric acid (LA, analytical grade, 98.5%), myristic
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acid (MA, analytical grade, 99%), hexadecanoic acid (HA, analytical grade, 99%) and
stearic acid (SA, analytical grade, 99%) were purchased from Chengdu Kelong
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Chemical Reagent Company (Chengdu, China). Wood-flour (WF, 325-mesh) was

supplied from Lingshou Shuolong mineral products processing factory. The
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wood-flour samples were dried at 105℃ for 4 h before use.

2.2. Preparation of FA/WF form-stable composite PCMs
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The FA/WF composite PCMs were prepared via a direct impregnation method. A
series of mass ratio of FA/WF composite were set as 4:6, 5:5 and 6:4 in order to
optimize the maximum absorption ratio without melted FA leaking from composites.
The beakers were sealed and put in the oven at 80 ℃ for 12 h, aiming for FA saturated
adsorption after FA/WF composite homogenized by stirring. Meanwhile, the FA/WF
composite in each beaker was stirred every 4 h during the adsorption process. Finally,
the samples were cooled down to room temperature. The FA/WF composite with the
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weight ratio of 6:4 was a bulk while the FA/WF composite with the weight ratio of
5:5 still maintained a powder, indicating the added fatty acid exceeded the absorption
capacity of WF. Thus the FA/WF composite with weight ratio of 5:5 was selected as
testing samples.
2.3. Characterization
2.3.1. Particle size and distribution
The particle size and distribution of WF were measured by MASTERIZER 2000

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(Malvern Instruments Ltd, England) at 25℃. The testing particle size ranges were

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from 0.02 to 2000 μm. Prior to testing process, WF was ultrasounding for 20 min to

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obtain a better dispersion in water.
2.3.2. Scanning election microscopy (SEM)

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The microstructures and morphologies of FA, WF and FA/WF composite were
observed using scanning electronic microscope (SEM, JEOLJSM-5900LV, Japan)
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with an accelerated voltage of 20 kV. The samples were gold-sputtered before the
observation.
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2.3.3. Fourier transform infrared spectroscopy (FTIR)

The structure of FA, WF and FA/WF composite were characterized using a Infrared
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Spectrophotometer (Nicolet-560, Nicolet Co., USA). The scanning range was

changed from 4000-400 cm-1 with a resolution setting of 4 cm-1. The KBr pressed disc
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technique (about 1 mg KBr of sample and 100 mg of KBr) was used to prepare the
test samples.
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2.3.4. X-ray diffraction (XRD)

The crystalline structures of FA, WF and FA/WF composite were studied by the
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X-ray diffraction (X’Pert pro MPD, Netherlands) with Cu Ka at 35 kV and 30 mA.

The scans were conducted in the 2θ ranging from 5° to 70° at a scanning rate of
0.04°/min.
2.3.5. Differential scanning calorimetry (DSC)
The DSC was employed to study the melting and freezing temperatures as well as
latent heat of LA and LA/WF composite using a differential scanning calorimeter
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(DSC 204 Phoenix, Netzsch, Germany) at a heating or cooling rate of 10℃/min under
nitrogen atmosphere. Before testing, the sample was heated from 40 to 100 °C and
kept at 100 °C for 2 min to eliminate the thermal history with the weight of all
samples about 8 mg.
2.3.5. Thermogravimetric analysis (TG)
The thermal stability of FA, WF and FA/WF composite was investigated on a
thermo-analyzer instrument (SDT-Q600, USA) under a nitrogen atmosphere. The

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mass of samples approximately 10 mg were placed into an aluminium oxide crucible

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and the heating/cooling rate of 10 °C /min from room temperature to 600℃.

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2.3.6. Accelerated thermal cycling testing
In order to confirm the thermal reliability, reusability and stability of FA/WF

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composite, accelerated thermal cycling test was conducted in high-low temperature
stages (STC200, Instec, USA) with 1000 consecutive thermal cycling from 0 to 100℃
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[12]. The time of thermal cycling program was set about 15 min for each
heating-cooling process. Afterwards, the phase change temperatures, latent heat and
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chemical stability of thermally treated FA/WF composite were characterized by DSC

and FTIR, respectively.
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3. Results and discussion

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3.1. Characterization of the support matrix

WF is selected as the supporting materials to synthetise the form-stab PCMs in this
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study. It is necessary to investigate the particle size and distribution of the pristine WF
before the FA/WF composite form-stable PCMs are prepared. The appearance feature
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of WF is shown in Fig. 1a. The average particle size and distribution of WF are shown
in Fig. 1b. As can be seen in Fig. 1a，the photography of WF presents the yellow flour.
In Fig. 1b, there is an apparently unimodal distribution in the particle size distribution
curve. The average particle size of WF is 58.5 μm, which is in agreement with that of
WF with 325-mesh approximately 44 μm. And the specific surface of WF is 0.33 m2/g,
which is contributed to absorbing the melting FA. Thus, WF is suitable to employ as
the supporting materials to prepare the FA/WF composite form- stable PCMs.
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3.2. Leakage test of FA/WF composite form-stable PCMs

In order to address the PCM leakage issues in building materials, it is essential to
conduct the leakage test of FA/WF composite form-stable PCMs. The photographs of
leakage test of WF, pure fatty acids and FA/WF composite form-stable PCMs are
displayed in Fig. 2. As shown in Fig. 2, the samples of WF, pure fatty acids and
FA/WF composite form-stable PCMs are pressed into small wafer. All wafers are
placed on a heating stage with increasing the temperature from 30 ℃ to 90 ℃ for 20

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min. It found that the pure fatty acids quickly meilted into liquid but WF and FA/WF

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composite form-stable PCMs can maintain the initial shape without liquid leaked

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during the whole heating process. Thus, the prepared FA/WF composite form-stable
PCMs have excellent form-stable performance with no leakage.

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3.3. Microstructure of WF and FA/WF composite form-stable PCMs
Fig. 3 and 4 show the morphologies and microstructures of WF and FA/WF
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composite form-stable PCMs before and after the absorption of FA. The Fig. 3 a and
b show the microstructures of WF with a typical fibrous materials. In Fig. 3a, the
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SEM of the pristine WF displays the irregular fiber fragments in a large magnification.
As shown in Fig. 3b, a great number of gully-like and tunnel-like veins are detected
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on the surface of WF, elaborating that the surface inhomogeneity and porosities of
WF can be filled by FA via the hydrogen-bond interaction, capillary force and surface
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tension force [43]. Compared with rough surface of WF, the surface of FA/WF
composite form-stable PCMs is smooth and locally even in Fig. 4. The porous spaces
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of WF are largely occupied by the impregnated FA, and less visible pores are
observed in the LW-FSPCM, MW-FSPCM, HW-FSPCM and SW-FSPCM, indicating
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the successful absorption of FA into WF. Hence, the FA/WF composite form-stable
PCMs manifest an potential for using in energy efficient buildings.
3.4. Chemical compatibility and crystalline property of FA/WF composite form-stable
PCMs
FTIR spectroscopy is carried out to to evaluate the probable interactions between
FA and WF during the composite process. The FTIR spectra of the WF, FA and
FA/WF composite PCMs is presented in Fig. 5. As seen from Fig. 5a, The FTIR
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spectrum of WF possesses the main absorption bands at 3380 cm-1 and 1031 cm-1 [42].
The peak around 3380 cm-1 correspondings to the O-H stretching vibration, and the
band at 1031 cm-1 is ascribed to the stretching vibration of C-O group. As for the
pristine LA, the characteristic peaks at 2917 cm-1 and 2845 cm-1 are attributed to C-H
stretching vibration of -CH3 and -CH2- groups. The characteristic absorption peaks of
the C=O stretching vibration and the C-O stretching vibration can be clearly observed
at 1702 cm-1 and 1303 cm-1. The corresponding O-H in-plane and out of plane

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vibration peaks of LA appear at 1430 cm-1 and 939 cm-1, respectively. Compared to

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the characteristic peaks of WF and LA, that of LW-FSPCM at 3380 cm-1 and 1031

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cm-1 is ascribed to characteristic absorption peaks of WF and that of LW-FSPCM at
2917 cm-1, 2845 cm-1, 1702 cm-1, 1430 cm-1, 1303 cm-1 and 939 cm-1 is attributed to

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characteristic absorption peaks of LA. This result demonstrates the existence of WF
and LA in the LW-FSPCM composite form-stable PCMs. Meanwhile, no additional
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characteristic absorption peaks appears in the FTIR spectra of LW-FSPCM, indicating
that there was no chemical reaction but only physical interactions between WF and
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LA. The similar results are obtained in the Fig. 5 b~d, meaning that there are also
only physical interactions between MA and WF, HA and WF, SA and WF.
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The XRD patterns of WF, FA and FA/WF composite form-stable PCMs are
displayed in Fig. 6. The crystalline structure of WF, FA and FA/WF composite
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form-stable PCMs is detected in fig. 6 a~d. As can be seen in Fig. 6a, the strong
diffraction peaks of WF appeared at 31.12°, 41.13°, 50.47°, and 51.37°, which is
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attributed to the crystalline cellulose that is naturally produced by a variety of

organisms (trees, plants, tunicates, algae, and bacteria) referring to as “natural”
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cellulose [47]. In Fig. 6a, the pure LA shows the sharp diffraction peaks at 21.79°,
and 24.31° due to its complete crystallization. As for LW-FSPCM, the characteristic
XRD peaks of the pure WF and LA are presented in that of LW-FSPCM. The
characteristic XRD peaks of WF are superimposed over that of LA. Therefore, no
new characteristic peaks of LW-FSPCM are observed in the XRD patterns, implying
that the crystal structures of the LA in the LA/WF composite form-stable PCM are not
affected by the direct impregnation treatment of WF.
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3.5. Phase change performances of FA/WF composite form-stable PCMs

It is very necessary to investigate the phase change properties such as phase change
temperature and latent heat of the excellent form-stable PCMs via DSC analysis. The
DSC curves of LA and LW-FSPCM, MA and MW-FSPCM, HA and HW-FSPCM,
and SA and SW-FSPCM are presented in Fig. 7 a~d. The detailed melting
temperatures, freezing temperatures and latent heats are included in Table 1. As
shown in Fig. 7a, the DSC curve of the LA/WF composite form-stable PCM exhibits

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similar curve with that of LA, meaning that the LA was mainly acted the role of the

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latent thermal energy storage during the phase change process. Furthermore, only a

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single and blunt peak of was observed in the melting and freezing curves, indicating
the phase change properties of LW-FSPCM were affected by adding WF due to the

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existence of the imperfect crystallites under the influence of WF. In table 1, the
melting temperatures and freezing temperatures of the pristine LA are measured as
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44.8℃and 41.3℃, and the melting and freezing latent heats of LA respectively reach
to 184.6 J/g and 179.2 J/g. Meanwhile, the melting and freezing temperatures and
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latent heats of LW-FSPCM exist at 40.2℃ and 42.6℃ as well as 87.9 J/g and 86.7 J/g,
respectively. The melting temperature of LA/WF composite is lower than that of pure
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LA, and the supercooling degree of 3.5℃ for the pure LA is higher than that of 1.4℃
for the LA/WF composite form-stable PCM, which is attributed to the reduction in
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crystal nucleus with the addition of WF [48]. Different from the supercooling degree
of LA and LW-FSPCM, the supercooling degree of 1.2℃ and 1.5℃ for MA and
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MW-FSPCM, the supercooling degree of 1.3℃ and 1.1℃ for HA and HW-FSPCM,
and the supercooling degree of 0.6℃ and 0.5℃ for SA and SW-FSPCM, are also
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detected in Table 1. The supercooling degree between MA and MW-FSPCM, HA and

HW-FSPCM and SA and SW-FSPCM, are almost same and still low. It also includes
that the melting atent heat of FA/WF composite form-stable PCM has identical with
freezing latent heats of those PCMs, implying that the WF has no effect on the
crystalline property of FA. The encapsulation ratio can be defined [49] by Formula (1)
on the basis of the heat of fusion obtained from the DSC analysis:
R= (ΔHm, FSPCM/ΔHm, FA) ×100% (1)
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Where: R is the weight percentage of LA in LA/WF composite form-stable PCMs;

ΔHm, FSPCM is the latent heat of LA/WF composite form-stable PCM, J/g; ΔHm, FA is
the latent heat of the pure FA, J/g. It can calculate that the encapsulation ratio of LA
in LA/WF composite form-stable PCMs arrives at 48.0%. Compared to that of
LW-FSPCM, encapsulation ratio of MW-FSPCM, HW-FSPCM and SW-FSPCM can
reach 50.7%, 51.6% and 48.6% respectively.
Table 2 indicates a comparison of thermal properties of prepared FA/WF composite

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form-stable PCMs with that of some wood-flour based form-stable PCMs in the

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literature. By comparison, the prepared LA-FSPCM, MW-FSPCM, HW-FSPCM and

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SW-FSPCM had a relatively higher latent heat than those reported composite PCMs,
especially the maximum latent heats in melting and freezing process for the

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HW-FSPCM can reach at 102.6 J/g and 103.5 J/g. Therefore, these FA/WF composite
form-stable PCMs can perfectly be utilized as thermal energy storage material in the
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energy efficiency building materials.
3.6. Thermal reliability of FA/WF composite form-stable PCMs
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It is indispensable to estimate the thermal reliability and reusability of PCMs for

the long time practical application via the accelerated thermal cycling process. The
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DSC curve of the prepared LA-FSPCM, MW-FSPCM, HW-FSPCM and SW-FSPCM

is shown in Fig. 8 a~d. The detailed melting and freezing latent heat before and after
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thermal cycling was displayed in Fig. 9, and the detailed melting and freezing point
before and after thermal cycling is shown in Fig. 10. As can be seen in Fig. 8 a~d, the
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DSC curve of the LW-FSPCM before and after thermal cycling exhibits hardly
change, manifesting that the crystalline property of FA in the FA/WF composite
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form-stable PCMs is no notably effect by the thermal cycling. In Fig. 9 a and b, the
melting and freezing latent heats of LW-FSPCM before and after thermal cycling are
87.9 J/g and 69.0 J/g as well as 87.7 J/g and 68.9 J/g, respectively. The average latent
heats loss ratio of LW-FSPCM arrives at 21.0%. However, the average latent heats
loss ratio of MW-FSPCM, HW-FSPCM and SW-FSPCM reached to 11.8%, 15.3%
and 6.4%, meaning that the thermal cycling has a negligible effect on latent heats of
FA/WF composite form-stable PCMs. As shown in Fig. 10 a and b, the melting and
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freezing point of LW-FSPCM before and after thermal cycling are 40.2 ℃ and 42.6 ℃
as well as 38.8 ℃ and 40.7 ℃, respectively. The melting and freezing point of
LW-FSPCM before and after thermal cycling remian unchanged. The similar results
of MW-FSPCM, HW-FSPCM and SW-FSPCM are also displayed in Fig. 10. In
conclusion, the prepared FA/WF composite form-stable PCMs can meet the thermal
reliability and reusability in practical application.
In order to further study the chemical structure change before and after thermal

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cycling, the FTIR spectra of LW-FSPCM, MW-FSPCM, HW-FSPCM and

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SW-FSPCM before and after 1000 thermal cycling is prepared in Fig. 11. As shown

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in Fig. 11, no additional new adsorption peaks occur. The original adsorption peak
positions and shapes are in agreement with after thermal cycling, confirming that the

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chemical structure can not change after thermal cycling. Therefore, the synthesized
FA/WF composite form-stable PCMs have good chemical stability.
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3.7. Thermal stability of FA/WF composite form-stable PCMs
The thermal stability of the FA/WF composite form-stable PCMs with different FA
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is investigated by TG analysis. Fig. 12 shows the TG curve of WF, FA and FA/WF

composite form-stable PCMs. As shown in Fig. 12, all samples are no apparently
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weight loss when the temperature is lower than 150℃. In Fig. 12a, it observes the
weight of WF sharply decreased to 62.7% once the temperature increases from 210 to
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380℃, and the weight of WF remains unchanged with further increasing the
temperature. The TG curve of the pure LA is similar to that of WF. The weight loss of
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LA mainly occurrs at the temperature between 150℃ and 235℃, and the weight of
LA is nearly invariable when further increased the temperature. As for LW-FSPCM,
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the first step is decomposition step corresponding to the thermal degradation of LA,
and the second step is attributed to the thermal degradation of WF. Compared to the
pure LA, the initial decomposition temperature of LW-FSPCM can enhance with
addition of WF, resulting from the strong intermolecular force [42]. The TG results
demonstrate that the prepared FA/WF composite form-stable PCMs have good
thermal stability in a broad phase transition temperature range of building materials
applications.
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4. Conclusion
The FA/WF composite form-stable PCMs have been successfully synthesized via a
direct impregnation method. SEM indicates that the porous spaces of WF can be
largely occupied by the impregnated FA, confirming WF can be acted as good support
matrixto prevent SA from leaking. FTIR and XRD results show that there was no
chemical reaction but only physical interactions between WF and FA. XRD analysis
also demonstrates that the WF has no effect on the crystallization of FA. DSC

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analysis shows that the supercooling degree between FA and FA/WF composite

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form-stable PCMs almost same and still low. Especially, the melting and freezing

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latent heat of HW-FSPCM and encapsulation ratio of HW-FSPCM can reach the
maximum value at 102.6 J/g and 103.5 J/g as well as 51.6%, indicating that the

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FA/WF composite form-stable PCMs are a preferred potential thermal energy storage
material for energy efficiency building applications. The results of thermal cycling
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demonstrate that the average melting and freezing latent heats loss ratio of
LW-FSPCM, MW-FSPCM, HW-FSPCM and SW-FSPCM reaches to 21.0%, 11.8%,
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15.3% and 6.4% with the minimum value at 6.4%, meaning that the FA/WF
composite form-stable PCMs had good thermal reliability and chemical stability. TG
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result reveals that the FA/WF composite form-stable PCMs have a good thermal
stability with the decomposition temperature of up to 150℃. Therefore, the prepared
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FA/WF composite form-stable PCMs have potential application in energy efficient

buildings for thermal energy storage.
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Conflict of interest statement:

We declare that we have no financial and personal relationships with other
people or organizations that can inappropriately influence our work, there is no
professional or other personal interest of any nature or kind in any product,
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service and/or company that could be construed as influencing the position

presented in, or the review of, the manuscript entitled, “Fabrication and
characterization of Fatty acid/wood-flour composites as novel form-stable phase
change materials for thermal energy storage”.

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Figure caption:
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Fig. 1 (a) photograph of WF; (b) particle size and distribution of WF.
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Fig. 2 Photographs of leakage test of WF, pure fatty acids and FA/WF composite
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Fig. 3 SEM images of WF: (a) ×100; (b) ×1000.

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Fig. 4 SEM images of FA/WF composite form-stable PCMs: (a) LW-FSPCM; (b)
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MW-FSPCM; (c) HW-FSPCM; (d) SW-FSPCM.

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Fig. 5 FTIR spectra of WF, FA and FA/WF composite form-stable PCMs: (a)
LW-FSPCM; (b) MW-FSPCM; (c) HW-FSPCM; (d) SW-FSPCM.
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Fig. 6 XRD diffractograms of WF, FA and FA/WF composite form-stable PCMs: (a)
LW-FSPCM; (b) MW-FSPCM; (c) HW-FSPCM; (d) SW-FSPCM.
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Fig. 7 DSC curves of pristine FA and FA/WF composite form-stable PCMs: (a) LA and
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SW-FSPCM.
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Fig. 8 DSC curves of FA/WF composite form-stable PCMs before and after thermal
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Fig. 9 Before and after thermal cycling of FA/WF composite form-stable PCMs: (a)
melting latent heat; (b) freezing latent heat.

Fig.10 Before and after thermal cycling of FA/WF composite form-stable PCMs: (a)
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melting point; (b) freezing point.

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Fig. 11 FTIR spectra of FA/WF composite form-stable PCMs before (solid line) and
after (dash dot dot line) thermal cycling: (a) LW-FSPCM; (b) MW-FSPCM; (c)
HW-FSPCM; (d) SW-FSPCM.
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Fig. 12 TG Curves of FA/WF composite form-stable PCMs: (a) LW-FSPCM; (b)
MW-FSPCM; (c) HW-FSPCM; (d) SW-FSPCM.
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Table 1 Latent heat storage properties of FA and the FA/WF composite form-stable
PCMs with the various FA contents

Melting process Freezing process

PCM
Tm (℃) ΔHm (J/g) Tf (℃) ΔHf (J/g)

LA 44.8 184.6 41.3 179.2

LW-FSPCM 40.2 87.9 42.6 86.7

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MA 52.1 198.2 53.3 193.3

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MW-FSPCM 51.2 99.6 52.7 98.7
HA 59.4 201.1 60.7 198.2

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HW-FSPCM 59.1 102.6 60.2 103.5
SA 52.0 192.3 52.6 187.7
SW-FSPCM 52.7
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Tm and Tf represented the melting and freezing point, respectively.

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ΔHm and ΔHf represented the melting and freezing latent heats, respectively.
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Table 2 Comparison of thermal properties of prepared FA/WF composite form-stable

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PCMs with that of some wood-flour based form-stable PCMs in the literature.

Melting process Freezing process

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Form-stable PCMs Refs

Tm (℃) ΔHm (J/g) Tf (℃) ΔHf (J/g)

lauric-myristic/CS-WF 33.1 98.2 32.8 96.1 [43]

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micro-encapsulated
16.7 45.9 7.9 44.3 [44]
paraffin/HDPE/WF
microencapsulated
22.2-28.7 31.6 --- 20.3 [45]
dodecanol/WF/HDPE
paraffin waxes/WF 26.18 20.62 --- --- [46]
lauric acid/WF 40.2 87.9 42.6 86.7 This work
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myristic acid/WF 51.2 99.6 52.7 98.7 This work

hexadecanoic acid/WF 59.1 102.6 60.2 103.5 This work
lauric acid/WF 52.7 92.7 52.2 92.1 This work

Tm and Tf represented the melting and freezing point, respectively.

ΔHm and ΔHf represented the melting and freezing latent heats, respectively.

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