2020-03-08 12:01:41
Bingmeng Li a, Dan Shu a, Ruifang Wang a, Lanlan Zhai a, Yuye Chai a, Yunjun Lan a, Hongwei Cao b, Chao Zou
1.Introduction
Since the 1970s, the energy and environmental problems have gradually aroused people’s attention. Therefore, people began to exploit renewable energy sources and improve energy efficiency. At present, the use of phase change materials (PCMs) is an effective way to store latent heat in the form of phase change enthalpy [1e4]. As one of the PCMs, PEG has been widely investigated for thermal storage due to its suitable phase change temperature, high latent heat capacity and high thermal and chemical stability after long- term utility period [2,5,6]. However, the leakage in the melting process has limited its applicability in energy storage [6e8].
One of the common solutions is to develop various supporting matrixes, such as polymers [7,9] and inorganic porous materials [6,10e17] to prevent the leakage of melted PEG. PEG/inorganic porous materials composites for energy storage have drawn great interest of researchers, since their thermal properties were better than those of PEG/polymer composites [18]. PEG/inorganic porous materials are usually prepared by physical methods such as ab- sorption blending, and impregnation [6,10e14,16,19]. Karaman et al. [15] prepared a form-stabilized PEG/diatomite composite PCM by vacuum impregnation method, and 50 wt% PEG was incorpo- rated into the pores of diatomite without any seepage. The melting
and freezing latent heats of the composite PCM were 87.09 J/g and 82.22 J/g, respectively. Zhang et al. [16] prepared PEG/silica sheets (GS) PCM by mixing GS with PEG at 70 ○C for 4 h. The highest enthalpy of the composite was 136.3 J/g and the mass fraction of PEG was 80 wt%. Wang et al. [6] prepared PEG/silica fume (SF) composites by physically blending after a series of complex pre- treatment of SF. The highest PEG loading was 47.9% and the highest value of enthalpy was 81.3 J/g. From these reports, the values of phase change enthalpy were rather low compared with that of pure PEG, which means the energy storage capacity of these PCMs was not desirable. Since PEG is absorbed into the pores by capillary force in the above investigations, the amount of PEG absorbed is significantly confined by the absorption capability of porous materials [12]. So the energy storage capability is influenced by the absorption capability of supporting materials.
To improve the absorption capability of supporting materials for higher phase change enthalpy and better energy storage capacity of PEG/porous materials, some measures were took during the syn- theses process, such as vacuum and outgassing. It was reported by Wang [20] that graphite was dried in a vacuum oven at 70 ○C for 20 h, and heated in a furnace at 900 ○C for 50 s. Then PEG/graphite blends were prepared by physically blending for 3 h. The maximum weight percentage of PEG was 90% with the latent heat of 161.2 J/g. Tian et al. [21] mixed PEG and methanol with silica gel (SG) which was outgassed for more than 3 h. The mixture was heated slowly in a water bath at 55 ○C about 9 h to obtain shape-stabilized PEG/SG composites. The pore fillingness of the composites was 80% and the highest enthalpy was 168.84 J/g. Though the enthalpy value of the composites and the mass fraction of PEG were improved after the pretreatment of porous materials, an amount of extra energy and time were consumed to increase the absorption capability of porous materials. Moreover, it was reported that the phase change enthalpy of PEG/porous materials was quantitatively correlated with the average pore diameter and the pore geometrical shape of the supporting materials [21e23] indicating that the absorption
capability essentially depends on the pore structure of porous materials. Pretreatments including vacuum and outgassing are not effective ways to improve the absorption capability of supporting materials, as the pore structure was ignored in the above reports. So the phase change enthalpy or the energy storage capacity of PEG/ porous materials cannot be efficiently increased, no matter how PEG was impregnated into the pore by these conventional syn- theses methods. Then the applications of PEG/porous materials in latent heat storage system are still restrained [24]. To avoid the influence of the absorption capability of porous materials, it has been widely reported that PCMs were encapsulated into SiO2 shell
by sol-gel method through hydrolysis and condensation [18,25e29]. However, most of these reports focused on n-alkane PCMs whose thermal properties are totally different from those of PEG. Moreover, surfactants and catalysts were adopted which have negative effect on the encapsulation ratio and encapsulation effi- ciency [27,28]. The values of the latent heat of the PCM@SiO2 composites decreased significantly in comparison of those of the corresponding pure PCMs.
Recently, the synthesis of mesoporous oxides using PEG sur- factant as structure-directing (templating) agent has been exten- sively studied and substantially reported [30e34], in which PEG is surrounded by hydrolyzable precursors, and then encapsulated into inorganic oxide framework during the process of hydrolysis and condensation. To obtain mesoporous structure, PEG usually needs to be calcined at high temperature or washed with solvents at the end of the synthesis process of mesoporous oxides. In this paper, PEG was packaged into silica framework to prepare PEG@-SiO2 composite in the light of the synthesis method of mesoporous silica without the elimination process of PEG. The mass fraction of the packaged PEG can be increased to the desired contents by the variation of the experimental conditions. The reported preparation by physical blending costs much more time (4 h-9 h) and higher temperature (55e70 ○C), with the pretreatment of vacuum or out-gassing for more than 3 h. In our work, the whole process of the preparation is much simple to operate at low cost without any pretreatment of supporting materials. PEG plays two roles during the preparation of PEG@SiO2, energy storage material and surfac- tant. Additional surfactant and catalyst were avoided, which will decrease the phase change enthalpy as foreign substance for the crystallization of PEG. This preparation method can eliminate the negative effect on both the absorption and the encapsulation of PEG. It benefits higher mass fraction of PEG and thus higher phase change enthalpy. Moreover, To the best of our knowledge, the preparation of PEG@SiO2 inspired by the synthesis of mesoporous materials as shape-stabilized PCM for energy storage has not been reported. The morphology, microstructure and thermal properties of the PEG@SiO2 were investigated by various techniques. Higher phase change enthalpy and energy storage capability of PEG@SiO2 were illustrated. PEG@SiO2 exhibited excellent thermal stability and reliability. Therefore, the facile synthesized composite with comprehensive properties is potential to be applied in energy storage devices such as solar-thermal energy conversion and stor- age systems.
2.Experimental section
2.1.Materials
PEG with an average molecular weight of 6000 (PEG 6000), tetraethoxysilane (TEOS) (>99%, GC grade) and isopropyl alcohol (IPA, 99.9%, GC grade) were purchased from Aladdin Reagent Co (Shanghai, China). N, N-dimethyl formamide (DMF) ( 99.5%, GC grade) was obtained from Guangdong Guanghua Sci-Tech Co, Ltd. Deionized water was used throughout the experiments.
2.2.Preparation of PEG@SiO2
PEG@SiO2 was prepared based on the common synthesis method of mesoporous silica. 5.30 g PEG, 8.64 g deionized water,
3.02 g DMF and 3.02 g IPA were mixed with the molar rate PEG: H2O: DMF: IPA 0.0184:10:0.86:1.05. The solution was then stirred vigorously for 0.5 h at room temperature. Thereafter, 10 g TEOS was added to the mixture under stirring for 1 h at room temperature. Afterwards, the products were washed by absolute ethanol five times and subsequently dried at 50 ○C for a week to completely eliminate the unencapsulated PEG and residual solvent. At last, the composite was obtained. The as-made bulk composite was calcined at 500 ○C for 5 h to obtain the supporting material for comparison.
The schematic illustration of preparation is shown in Fig. 1.
2.3.Sample characterization
Morphological analysis was undertaken using SEM (FEI Nova Nano SEM 200). Energy dispersive X-ray spectroscopy (EDS) coupled with SEM was used to analyze the chemical composition. High-resolution transmission electron microscopy (HRTEM), high- angle annular dark-field (HAADF), scanning transmission electron microscopy (STEM), and EDS were performed on JEOL 2100F mi- croscope. Composition analysis was performed by EDS (oxford INCA). The samples for TEM and STEM-EDS were collected by placing a drop of sample dispersed in absolute ethanol onto carbon- film-supported copper grids. The surface areas, pore volume and pore size distribution of the calcined sample were determined at 77 K using a BELSORP-mini II instrument (Bel Japan Inc.). The calculation of pore size was performed using the Bar- retteJoynereHalenda (BJH) method applied to the adsorption data of the N2 sorption isotherms. An FT-IR spectrometer (Perkin Elmer, USA) was used to characterize the prepared composite. The crystal structures and crystallization properties were studied using wide angle X-ray diffraction (WAXD) (Bruker, D8 advance, Cu Ka radiation using a curved graphite receiving monochromate), with a step of 0.02○ at a speed of 4○/min from 10○ to 80○ at room temperature.
Differential scanning calorimetry (DSC) was carried out to measure the phase change temperature and enthalpy of the samples using Q1000 (TA Instrument, USA) at heating/cooling rate of 10 ○C/min from 10 ○C to 110 ○C in nitrogen atmosphere. The thermal analysis was performed by a thermogravimetric analysis Diamond TG-DTA/Spectrum GX (Perkin Elmer, USA) in nitrogen atmosphere and ox- ygen atmosphere, respectively. The samples were scanned over the temperature range from room temperature to 800 ○C at a heating rate of 10 ○C/min.
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