现代化工

现代化工 ›› 2025, Vol. 45 ›› Issue (S1) : 200-204. DOI: 10.16606/j.cnki.issn0253-4320.2025.S1.037

科研与开发

石蜡/SiO₂/mEG相变材料的制备与热性能探究

张豪 ¹ ,
曹姗姗 ¹^,^* ,
齐承英 ¹ ,
吴向东 ²

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Preparation and thermal properties of paraffin/SiO₂/mEG phase change materials

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文章历史 +

Received		Published
2024-06-03		2025-05-30
Issue Date	Revised Date
2025-05-23	2024-06-03

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摘要

为了提高石蜡(PW)的导热性能和改善泄露问题,研究了一种混合尺寸膨胀石墨(mEG)和纳米二氧化硅(SiO₂)协同的体系。采用浸渍法制备了一种新型形状稳定的PW/SiO₂/mEG复合相变材料,并对复合相变材料的热性能、微观结构、循环稳定性等进行了研究。结果表明,制备的PW/SiO₂/EG-20目-18 μm具有丰富的三维吸附网络,对PW吸附效果显著;在110℃及以下温度可实现无泄漏储热,并具有良好的形态稳定性;mEG极大地提高了相变材料的传热性能;10% EG-20目-18 μm的加入使得PW/SiO₂/mEG的导热系数提升为4.05 W/(m·K),较纯石蜡提高了约13.1倍;此外,还观察到PW/SiO₂/EG-20目-18 μm在经历300次熔融和凝固循环后相变温度仅变化了0.3℃,潜热降低了2.20 J/g,表现出良好的热循环稳定性。

Abstract

In order to enhance the thermal conductivity paraffin wax (PW) and solve its leakage problem,a synergistic system comprising hybrid size-expanded graphite (mEG) and silicon dioxide (SiO₂) nanoparticles is developed.A novel shape-stable PW/SiO₂/mEG composite phase change material is prepared via the impregnation method,and its thermal properties,microstructure,and cycling stability are studied.Results show that the prepared PW/SiO₂/EG-20 mesh-18 μm has a rich three-dimensional adsorption network and presents a great adsorption effect for PW.It is shown that the prepared PW/SiO₂/EG-20 mesh-18 μm can achieve leak-free thermal storage at 110℃ and below temperature,showing good morphological stability.mEG greatly improves the heat transfer performance of the phase change material.The addition of 10 wt% EG-20 mesh-18 μm enhances the thermal conductivity of PW/SiO₂/mEG to 4.05 W/(m·K),which is about 14.1 times that of pure paraffin.In addition,it is also observed that the phase transition temperature of PW/SiO₂/EG-20 mesh-18 μm sample only changes by 0.3℃ and the latent heat decreases by 2.20 J·g^-1 after 300 cycles of melting and solidification,showing good thermal cyclability.

Graphical abstract

关键词

复合定型相变材料 / 热性能 / 混合尺寸膨胀石墨 / 纳米二氧化硅 / 石蜡

Key words

composite shaped phase change materials / thermal performance / hybrid size-expanded graphite / SiO₂ nanoparticles / paraffin

Author summay

张豪(2000-),男,硕士生,研究方向为多能互补及优化利用技术,202221302010@stu.hebut.edu.cn。

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随着现代社会能源需求的不断增加,供需不匹配的问题日益严重,迫切需要探索高效的能源储存方法^[1]。热能存储(TES)是提高能源利用率和降低能耗的重要措施^[2]。其中,应用相变材料(PCM)进行潜热储存是热能存储最有效的方法,因为它能够在相变过程中储存大量能量^[3]。常用的相变材料包括石蜡(PW)、脂肪酸和水合盐等。其中,PW因具有价格低廉、无腐蚀性、过冷度低等特性,而得到了广泛的应用^[4],但低导热和易泄露等问题限制了其进一步的应用^[5]。

膨胀石墨(EG)因其价格低廉、导热性好、孔隙丰富、制造简单等特点,被广泛应用于提升PW的形状稳定性和导热性。相关研究^[6]表明EG增强传热效果明显,同时可保证复合相变材料(CPCM)的形状稳定性。周丽等^[7]通过真空浸渍法制备了膨胀石墨-石蜡复合相变储能材料,当膨胀石墨的质量分数为12%时,复合相变储能材料的导热系数约为3.25 W/(m·K),但存在较多泄露;继续提高膨胀石墨的添加比例至15%,仍然存在较多泄露现象。类似的情况在脂肪酸^[8]和醇类有机共晶复合物^[9]等相变材料中也存在。泄露使PCM从EG基体中析出,长期的泄露甚至会导致分层现象,严重影响储热效果。虽然EG多孔基体可在相变材料内部形成吸附网络,缓解PCM的渗漏问题^[10],但当吸附达到饱和状态,继续添加EG对PCM的吸附效果影响较小,因此,有必要进一步提高基于EG为基体的防泄漏性能。田云峰等^[11]发现两种不同粒径的EG配合可以形成镶嵌网络,达到更好的吸附效果,但对于粒径的选择问题并未研究。此外,SiO₂因具有较大的比表面积也常被用来吸附固-液相变材料,且具有优秀的防漏效果和优异的循环可靠性^[12]。

因此,本文建立了以不同粒径搭配的膨胀石墨(mEG)为载体、SiO₂为吸附剂的吸附体系,与PW相变材料制备了复合定形相变材料,并通过热性能测试、微观结构观察、热循环性测试等检验其性能,探究mEG的不同粒径搭配对PCM性能的影响,旨在提高PCM的整体导热性和减少泄漏。

1 实验

1.1 材料

PW单体(PCM-A-58H)购自广州中佳相变材料有限公司;纳米SiO₂(吸附剂,平均粒径10 nm,比表面积380 m²/g,类球形,白色)购自上海肴戈合金材料有限公司;膨胀石墨(吸附剂,导热添加剂,粒度20目、100目、18 μm,灰分≤0.2%,膨胀体积 400~600 mL/g)购自青海岩海碳材料有限公司。

1.2 PW/SiO₂/mEG的制备

PW/SiO₂/mEG的制备如图1所示。首先,将预定质量的PW放置在烧杯中,并在90℃的温度下恒温加热30 min,确保PW完全熔化;为了使SiO₂分布均匀,将SiO₂放入烧杯中与熔融PW混合,并使用搅拌子高速磁力搅拌30 min;向熔融物中添加一定比例的小粒径膨胀石墨1(EG-min),使用磁力搅拌子进行30 min的搅拌,使纳米SiO₂和PW均匀分布于EG-min微孔中;再加入一定比例的大粒径膨胀石墨2(EG-max)并使用玻璃棒进行30 min的搅拌,确保添加物混合均匀;最后,用小勺取出最终制品放入圆形模具中,用压片机以10 kg的力压制成型,待冷却至室温,PW/SiO₂/mEG样品制作完成。

优先制备了质量分数0.8% SiO₂的样品W0,后分别与mEG(EG-20目-18 μm、EG-20目-100目、EG-100目-18 μm)以一定的比例制备了复合相变材料W1、W2和W3,配比如表1所示。

2 表征

采用傅里叶变换红外光谱仪(Bomem SRG1100G S/N)在400~4 000 cm^-1的波长范围内,以4 cm^-1分辨率表征CPCMs的化学相容性。采用场发生扫描电子显微镜(FESEM)对样品的微观结构进行表征。使用差示扫描量热仪(DSC,204 F1型,德国耐驰),在氮气流速为50 mL/min、实验温度为0~150.00℃、加热速率为10℃/min的条件下,测定了CPCMs的热性能。使用热常数分析仪(Hot Disk TPS 2500S,瑞典),通过瞬态平面热源法测量CPCMs在室温下的热导率。

3 结果与讨论

3.1 DSC分析

图2为PW和W0的DSC曲线。由图2可知,W0的DSC曲线因添加了质量分数0.8%的SiO₂而向高温偏移,焓值没有明显变化。PW在熔融过程中的相变温度为57.3℃,W0的相变温度较纯PW高出1.3℃。原因是由于SiO₂中存在着表面吸附力等微观力使W0熔化延迟^[13]。

样品W1~W3的DSC测试结果见图3。由图3可知,W1~W3相变区间较W0没有出现明显的偏移,样品W1~W3的熔融潜热较理论值210.8 J/g也相差不大。因此,mEG的加入对PW/SiO₂的焓值和相变温度无明显影响。

3.2 FT-IR

PW、SiO₂、EG、PW/SiO₂、PW/SiO₂/mEG的 FT-IR谱图如图4所示。PW在波长2 926、2 911 cm^-1和2 852 cm^-1处的特征峰分别是由—CH₃及—CH₂中的C—H单键的拉伸振动引起的^[14]。而1 472 cm^-1和1 629 cm^-1的特征峰分别对应于C—H单键的弯曲振动和伸缩振动^[15]。此外,在730 cm^-1处出现—CH₂的摇摆振动吸收峰^[16]。在EG光谱中,两种不同规格的EG曲线相似。在 3 438 cm^-1的吸收峰是由H—O—H单键的弯曲振动引起的。在2 918 cm^-1的吸收峰是由—CH₂的反对称伸缩振动引起的^[17],在1 632 cm^-1的吸收峰与吸附水分后的弯曲振动有关^[18]。SiO₂在3 445 cm^-1和1 636 cm^-1处的特征峰是由羟基的拉伸振动引起的^[19]。此外,在1 065 cm^-1和473 cm^-1处观察到的吸收峰,分别是Si—O—Si的不对称拉伸振动和弯曲振动。由PW-SiO₂的FT-IR吸收谱图可以看出,PW-SiO₂与PW和SiO₂具有相似的吸收峰,但是在468 cm^-1和1 057 cm^-1处的Si—O—Si吸收峰有所减弱,这是因为SiO₂的含量较低。此外,PW、SiO₂、EG-20目、EG-18 μm的吸收峰也都存在于PW/SiO₂/EG-20目-18 μm的曲线上,未观察到新的特征峰。该结果表明材料之间的作用力为物理吸附,没有发生化学反应,也没有产生新物质。

3.3 微观结构和形貌分析

图5描绘了SiO₂、PW/SiO₂、EG、PW/SiO₂/mEG断裂面的微观结构和形貌特征。从图5(a)可见,SiO₂微观结构为絮状球体;图5(b)可知,含有质量分数0.8% SiO₂的PW/SiO₂体系中的SiO₂纳米颗粒分布均匀;图5(c)~5(e)中,EG粒径依次减小,EG-20目依然保持蠕虫状,EG-18 μm即为粉碎状。从图5(f)~5(h)可以看出,PW/SiO₂/EG-20目-18 μm表面充实,质地紧密,复合效果好。这主要是因为SiO₂纳米颗粒和EG-18 μm可与PW一同填补于EG-20目的空隙中,内部形成SiO₂、EG-18 μm、EG-20目三重吸附,使内部吸附网络更加丰富,结构更加稳固。PW/SiO₂/EG-20目-100目断裂面呈现颗粒状且结构松散,这种现象可能是由于EG-20目与EG-100目镶嵌效果差导致的,EG-20目和EG-100目吸附PW后镶嵌不完全而进行堆叠,最终形成块状结合体。PW/SiO₂/EG-100目-18 μm样品表面呈现出与PW相似的微观特性,这是由于SiO₂和EG-100目-18 μm组成的吸附网络难以完全吸附PW,当PW完全填充EG蜂窝孔时,多余的PW会粘附在EG表面。

3.4 形态稳定性及泄露特性分析

对PW/SiO₂/mEG复合物进行热处理,以检查形状稳定性和泄漏性。选取两块相同配比的PW/SiO₂/mEG为一组,在不同的温度下恒温加热 5 h,待自然冷却至室温,记录加热前后的质量变化和形态变化。由于W3在热处理后泄露严重,故不再做泄露分析。W1、W2泄露结果如图6所示。由图6可知,W1和W2的泄露率随着加热温度的升高呈现先平稳后上升的趋势。这主要是因为PW的熔化体积随温度的升高而增大,因此升高到一定的温度后,PW的总体积会突破mEG和SiO₂体系的吸附阈值,从而泄露开始增加。在同等温度下,W1的泄露率始终低于W2,这得益于W1体系中 EG-18 μm和EG-20与SiO₂纳米颗粒的镶嵌结构,形成由内到外的三重吸附作用,保证PW结构紧密,不易泄露。W1和W2在热处理后虽都有一定的泄露,但形貌几乎没有变化,以150℃加热前后的形态图为参考,见图7。综上,mEG的添加对PW的形貌稳定性和防泄露均有所提高,但因mEG的组成成分不同,表现出的效果有所差异。其中W1在保持形态稳定性的同时拥有优秀的防泄漏性,在110℃以下泄漏率<0.3%,对于低温领域的无泄漏储热研究具有重大意义。

3.5 导热性能分析

图8显示了复合相变材料的热导系数测试结果。由图可知,添加0.8%的SiO₂纳米颗粒后,W0导热系数达到了0.295 W/(m·K),相较纯PW提高约2.5%。这表明SiO₂不仅在吸附和成型中起了作用,而且略微增强了PW的导热系数,而这种热导率的增强可归因于SiO₂的均匀分散为热传导提供了更好的路径。当添加10%的EG-20目-18 μm、EG-20目-100目和EG-100目-18 μm后,W1、W2和W3的导热系数相较于纯PW分别提升了13.1、12.4倍和2.9倍。这表明mEG可大幅度提升PCM的导热系数,但受到尺寸搭配的影响较大,mEG中EG-max粒径的增大和EG-min粒径的减小均有利于导热性能的提升。其中,EG-20目与EG-18 μm的搭配使用增强导热性能最佳。因此,在工程实践中,需要综合考虑应用要求和实际材料性能,合理选择mEG的尺寸搭配。

3.6 循环稳定性分析

由于W1在以上测试中均表现良好,因此本节选用W1测试其循环稳定性,结果见图9。由图9可知,W1在经历了300次储热循环后的DSC曲线与循环前并无明显变化。循环后的熔化温度升高了0.3℃,潜热降低了2.20 J/g,两者均变化较小。由此可见,W1在实际储热/释放循环应用中相变温度和相变潜热可基本保持稳定,具有优异的化学和晶体结构稳定性,可在较长时间内稳定使用。

4 结论

(1)mEG和SiO₂的协同吸附体系效果显著,使得W1在各种测试温度下都具有良好的形态稳定性,且在一定温度下具有良好的防漏性能。W1在110℃以下泄漏率<0.3%,可作为低温储热的候选材料。

(2)mEG的镶嵌协同结构具有优秀的导热增强作用。由EG-20目-18 μm制备的W1的导热系数达到了4.053 W/(m·K),较纯PW提高了约13.1倍。导热系数受mEG中EG粒径组合的调控,EG-max粒径的增大和EG-min粒径的减小均有利于导热性能的提升。因此可根据实际需要,合理选择mEG的尺寸搭配。

(3)W1在300次熔融和凝固循环后相变温度变化了0.3℃,潜热降低了2.20 J/g,说明PW/SiO₂/EG-20目-18 μm具有良好的循环稳定性。

本研究使用SiO₂和mEG吸附体系制备了一种新型防泄漏的低温高导热储热定型相变材料,并研究得出mEG的最佳粒径搭配,提供优秀导热性能的同时减少泄露。研究为后续mEG的使用提供理论数据支撑。但不足之处在于本研究的mEG只由两种不同尺寸的EG组成,未来还需进一步对更多mEG进行研究,以此来探究其潜在应用价值。

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