Preparation of highly thermally conductive and shape-stabilized polyethylene glycol-based phase change material

doi:10.11949/0438-1157.20221141

Abstract

Abstract:

Shape-stabilized and highly thermally conductive phase change materials (PCMs) have been prepared based on polyethylene glycol (PEG) and boron nitride (BN). The PCMs are obtained by two-step blending assisted by the complexation of polyacrylic acid (PAA). The thermal conductivity and the stabilization mechanism of the PCMs have been investigated. The results show that the flake-like BN can significant improve the thermal conductivity of the composites. The thermal conductivity of the prepared PCMs can reach to 6.437 W/(m·K) when the mass fraction of BN is 60%. It is also confirmed that when one-third and one-sixth of flake-like BN is replaced by the spherical BN, the composites show an increased thermal conductivity, which suggests that the hybrid fillers has positive effect on the enhancement of thermal conductivity. The experimental results demonstrate that PAA can form hydrogen bond with PEG, which contributes to preventing the leakage of PEG from the matrix when enduring heating. In addition, abundant flake-like BN can act as a solid physical barriers to restrict the molten PEG being escaped from the matrix, resulting the excellent shape preserving property.

Key words: composites, phase change, polymers, heat conduction, boron nitride

摘要：

利用聚乙二醇为相变组分，以氮化硼为导热填料，通过两步法络合聚丙烯酸制备了具有相变稳定性的高导热相变复合材料。系统研究了片状氮化硼以及片状/球形混杂填充对复合材料导热以及相变性能的影响，探讨了相变复合材料的定形机理。结果表明，由于紧密的堆砌结构，片状氮化硼能够有效提升复合材料导热性能。填充60%（质量）的片状氮化硼时，热导率最高达到6.437 W/(m·K)。在混杂填充时，球形氮化硼与片状氮化硼的质量比为1∶3以及1∶6时，可以更加有效提升复合材料的导热性能。热储存实验显示，所制备的复合材料具有良好的热存储能力。此外，由于聚丙烯酸与聚乙二醇形成氢键的络合以及氮化硼的片状物理阻隔作用，复合材料在高温加热条件下具有优异的相变稳定性。

关键词: 复合材料, 相变, 聚合物, 热传导, 氮化硼

CLC Number:

TQ 316.6

Wenqi CUI, Shuguang YANG, Hongzhou LI, Fubin LUO. Preparation of highly thermally conductive and shape-stabilized polyethylene glycol-based phase change material[J]. CIESC Journal, 2022, 73(12): 5660-5671.

崔雯琦, 杨曙光, 李红周, 罗富彬. 聚乙二醇高导热定形相变复合材料的制备及其性能研究[J]. 化工学报, 2022, 73(12): 5660-5671.

Figures/Tables 13

Table 1 The mass ratio of PEG， PAA and BN in the composites

Sample	PEG质量/g	PAA质量/g	PEG与PAA的质量比	f-BN质量/g	s-BN质量/g	f-BN与s-BN的质量比
PCM-(PEG₃/PAA₁)-(f-BN₃/s-BN₁)	30.0	10.0	3∶1	45.0	15.0	3∶1
PCM-(PEG₆/PAA₁)-(f-BN₆/s-BN₁)	34.3	5.7	6∶1	51.4	8.6	6∶1
PCM-(PEG₉/PAA₁)-(f-BN₉/s-BN₁)	36.0	4.0	9∶1	54.0	6.0	9∶1
PCM-(PEG₁₂/PAA₁)-(f-BN₁₂/s-BN₁)	36.9	3.1	12∶1	55.4	4.6	12∶1
PCM-(PEG₃/PAA₁)-(f-BN-60)	30.0	10.0	3∶1	60.0	0
PCM-(PEG₆/PAA₁)-(f-BN-60)	34.3	5.7	6∶1	60.0	0
PCM-(PEG₉/PAA₁)-(f-BN-60)	36.0	4.0	9∶1	60.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-60)	36.9	3.1	12∶1	60.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-40)	55.4	4.6	12∶1	40.0	0
PCM-(PEG₁₂/PAA₁)-(f-BN-20)	73.8	6.2	12∶1	20.0	0

Fig.1 SEM images of flake-like boron nitride (a) and spherical boron nitride (b)

Fig.2 Thermal conductivity of the PCM composites filled with 60%(mass) flake-like boron nitride (a), flake-like/spherical boron nitride hybrids (b) and different content of flake-like boron nitride (c), respectively

Fig.3 SEM images of PCM composites filled with flake-like/spherical boron nitride hybrids: (a) s-BN∶f-BN=1∶3, (b) s-BN∶f-BN=1∶6, (c) s-BN∶f-BN=1∶9, (d) s-BN∶f-BN=1∶12；Schematic diagram of thermally conductive paths: (e) s-BN∶f-BN=1∶6, (e) s-BN∶f-BN=1∶12

Fig.4 DSC curves of the PCM composites filled with flake-like boron nitride (a) and flake-like/spherical boron nitride hybrids (b)

Table 2 Phase transformation enthalpy and phase transition temperature of the prepared PCM composites filled with flake-like boron nitride

Sample	T_m/℃	ΔH_m/(J/g)	Theoretical Δ H_m/(J/g)	T_c/℃	ΔH_c/(J/g)	Theoretical Δ H_c/(J/g)
PEG	58.93	141.2		39.48	139.5
PCM-(PEG₃/PAA₁)-(f-BN-60)	53.63	33.91	42.36	—	—	41.85
PCM-(PEG₆/PAA₁)-(f-BN-60)	58.42	40.18	48.41	24.28	37.44	47.83
PCM-(PEG₉/PAA₁)-(f-BN-60)	57.69	50.70	50.83	32.55	49.88	50.22
PCM-(PEG₁₂/PAA₁)-(f-BN-60)	57.93	51.07	52.14	35.84	47.65	51.51
PCM-(PEG₁₂/PAA₁)-(f-BN-40)	56.70	90.94	78.22	30.93	87.45	77.28
PCM-(PEG₁₂/PAA₁)-(f-BN-20)	58.08	119.1	104.21	36.19	119.0	102.95

Table 3 Phase transformation enthalpy and phase transition temperature of the prepared PCM composites filled with flake-like/spherical boron nitride hybrids （60%）

Sample	T_m/℃	Δ H_m/(J/g)	Theoretical Δ H_m/(J/g)	T_c/℃	Δ H_c/(J/g)	Theoretical Δ H_c/(J/g)
PCM-(PEG₃/PAA₁)-(f-BN₃/s-BN₁)	58.51	28.69	42.36	—	—	41.85
PCM-(PEG₆/PAA₁)-(f-BN₆/s-BN₁)	58.83	37.43	48.41	24.56	35.89	47.83
PCM-(PEG₉/PAA₁)-(f-BN₉/s-BN₁)	53.83	32.72	50.83	24.57	32.97	50.22
PCM-(PEG₁₂/PAA₁)-(f-BN₁₂/s-BN₁)	55.34	40.17	52.14	30.28	39.48	51.51

Fig.5 XRD patterns of the PCM composites filled with flake-like boron nitride [(b) is the enlarged view of the zone marked by dotted lines in (a)]

Fig.6 The shape stability performance of the prepared PCM composites: (a) digital pictures of the specimens upon heating (100℃); (b) digital pictures of the specimens upon heating and cooling cycles at 80℃ [the specimen codes (1), (2), (3) and (4) represent the PCM composite containing a PAA /PEG ratio of 1∶3, 1∶6, 1∶9, 1∶12, respectively, corresponding to PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG6/PAA1)-(f-BN-60), PCM-(PEG9/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), the specimen code (5) refers to the PEG/f-BN PCM composite]

Fig.7 The shape stability performance of the prepared PCM composites: (a) digital pictures of the specimens upon heating (100℃); (b) digital pictures of the specimens upon heating and cooling cycles at 80℃ [the specimen codes (6), (7) and (8) represent the PCM composite filled with 20%(mass), 40%(mass) and 60%(mass) f-BN respectively, corresponding to PCM-(PEG12/PAA1)-(f-BN-20)，PCM-(PEG12/PAA1)-(f-BN-40) and PCM-(PEG12/PAA1)-(f-BN-60)]

Fig.8 FTIR of the PCM composites (a), SEM of the PCM composites (b), where (1), (2), (3) and (4) corresponding to PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG6/PAA1)-(f-BN-60), PCM-(PEG9/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), respectively; shape stabilized mechanism diagram of the PCM composite (c)

Table 4 Comparison of polyethylene glycol-based thermally conductive phase change composites reported in literature

编号	填充组分	填料比例	定形以及制备方式	热导率/（W/(m·K))	文献
1	膨胀石墨/改性云母	3.22%(质量)/32.25%(质量)	多孔石墨定形，真空浸渍法	0.56	[34]
2	银纳米线/膨胀蛭石	19.3%(质量)/21.9%(质量)	膨胀蛭石定形，物理共混和浸渍法	0.68	[25]
3	氮化硼/石墨烯	23%(质量)/少量	冰模板自组装氮化硼/石墨烯多孔类气凝胶定形，真空浸渍法	2.36	[29]
4	硅藻土/碳纳米管	36.8%(质量)/3.2%(质量)	硅藻土孔结构定形，浸渍法	1.52	[35]
5	改性二氧化硅/氧化碳纳米管	39.4%(质量)/0.6%(质量)	改性二氧化硅定形，溶胶-凝胶法	0.41	[36]
6	氮化硼/纳米纤维素/壳聚糖	47.4%(质量)/15.8%(质量)/2.4%(质量)	纳米纤维素/壳聚糖界面相互作用定形，界面聚电解质络合纺丝法	4.005	[37]
7	二氧化硅/石墨	10%(质量)/6%(质量)	二氧化硅网状分子结构定形，溶胶-凝胶法和浸渍法	1.867	[38]
8	聚丙烯酰胺	40%(质量)	聚丙烯酰胺三维网络结构定形,化学交联法	0.375	[39]
9	氮化硼/聚丙烯酸	60%(质量)/3.1%(质量)	片状氮化硼阻隔及聚丙烯酸氢键络合，熔融共混浇筑法	6.437	本文

Fig.9 Surface temperature variation curves of E51/BN, PEG/PAA, PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60) samples recorded by an infrared imaging devices upon heating (a); the diagram of the testing experiment (b); infrared thermal imaging of four samples upon heating (c); where (T-1), (T-2), (T-3), (T-4) are corresponding to PEG/PAA, PCM-(PEG3/PAA1)-(f-BN-60), PCM-(PEG12/PAA1)-(f-BN-60), E51/BN, PEG/PAA, respectively

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