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氧化铝(Al_2O3)纳米纤维作为一种性能优异的高温隔热材料,在航空航天、消防救援等领域具有广阔的应用前景。然而,Al_2O3纤维在高温晶型转变过程中易发生晶粒快速生长,导致纤维脆化开裂,限制其实际应用。元素掺杂是抑制晶粒过度生长、改善Al_2O3基纤维膜高温柔性失效问题的有效途径。本文结合溶胶-凝胶法与静电纺丝技术,通过引入Zr、Si掺杂元素,成功制备出具有良好柔性的二维Al_2O3基纳米纤维膜。利用扫描电镜(SEM)、透射电镜(TEM)和X射线衍射(XRD)等手段,系统研究了掺杂元素种类、掺杂比例及煅烧温度对纤维形貌与晶体结构的影响,并对纤维膜的拉伸强度、弯曲性能等力学性能进行了系统表征。结果表明,引入Zr元素掺杂可使纤维晶粒尺寸显著降低,同时提升其柔韧性,但该纤维膜经1 400℃高温煅烧后,出现晶粒粗化现象,并导致柔韧性显著下降。当掺杂元素为Si、铝硅摩尔比为6∶1时,所得Al_2O3-SiO2纳米纤维膜形貌均匀,晶体结构为稳定的莫来石相。该纤维膜在1 400℃煅烧后仍保持良好的柔性;经1 000℃煅烧后,其拉伸强度达1.03 MPa,500次弯折循环后弯曲刚度仍保持在70 mN,室温导热系数较低(0.029 9 W/(m·K)),表现出优异的综合性能。
Abstract:Alumina(Al_2O3) nanofiber membranes are promising high-temperature thermal insulation materials with broad applications in aerospace, firefighting, and rescue operations. However, rapid grain growth during phase transformation tends to cause brittle cracking, limiting their practical use. Element doping is an effective strategy to suppress excessive grain growth and improve the high-temperature flexibility of Al_2O3-based fiber membranes. In this study,two-dimensional Al_2O3-based nanofiber membranes with good flexibility were fabricated by combining sol-gel and electrospinning techniques with the incorporation of Zr and Si as dopants. Scanning electron microscopy(SEM), transmission electron microscopy(TEM), and X-ray diffraction(XRD) were employed to investigate the effects of dopant type, doping ratio, and calcination temperature on fiber morphology and crystal structure. Tensile strength and flexural performance were also systematically characterized. The results show that Zr doping significantly reduces grain size and improves flexibility. However, calcination at 1 400 °C leads to noticeable grain coarsening and a marked decline in flexibility. In contrast, when Si is used as the dopant at an Al ∶Si molar ratio of 6 ∶1, the resulting Al2 O3-SiO2 nanofiber membrane exhibits uniform morphology and a stable mullite phase. This membrane retains good flexibility after calcination at 1 400 ℃. After calcination at 1 000 ℃, it achieves a tensile strength of 1.03 MPa, maintains a flexural stiffness of 70 mN after 500 bending cycles, and shows a low room-temperature thermal conductivity of0.029 9 W/(m·K), demonstrating excellent overall performance.
[1]孙凡惠,杨金,郑敏博,等.热防护功能纤维与智能纺织品的研究进展[J].科学通报,2025, 70(17):2718-2732.SUN F H, YANG J, ZHENG M B, et al. Research progress on functional fibers and smart textiles for thermal protection[J]. Chinese Science Bulletin, 2025, 70(17):2718-2732.(in Chinese)
[2]郝栋连,冯慧,苏悦,等.高温隔热材料的研究现状及发展趋势[J].合成纤维工业,2022, 45(1):68-73.HAO D L, FENG H, SU Y, et al. Research status and development trend of high temperature thermal insulation materials[J]. China Synthetic Fiber Industry , 2022 , 45(1):68-73.(in Chinese)
[3]DING Y, LIU T, JIANG Y, et al. Flexible fire-resistant and heat-insulating materials fabricated using sodium titanate nanobelts[J]. Materials Today Nano , 2022 , 17:100161.
[4]郭晗.柔性莫来石/莫来石-氧化锆复合纳米纤维的制备及其性能研究[D].北京:北京化工大学,2024.GUO H. Preparation and performance study of flexible mullite/mullite zirconia composite nanofibers[D]. Beijing:Beijing University of Chemical Technology, 2024.(in Chinese)
[5]ZHANG J, ZHANG X, WANG L F, et al. Fabrication and applications of ceramic-based nanofiber materials service in high-temperature harsh conditions:a review[J]. Gels ,2023, 9(3):208.
[6]LIU H Y, WU N, ZHANG X S, et al. Research progress on electrospun high-strength micro/nano ceramic fibers[J].Ceramics International, 2022, 48(23):34169-34183.
[7]LI J, RUI J M, LI Y J, et al. Zr-doped SiOC ceramics fibers and the high-temperature thermal performance[J].International Journal of Applied Ceramic Technology,2023, 20(4):2438-2448.
[8]杨朝坤,华永明,花拓.隔热纤维材料的隔热机理及其应用[J].棉纺织技术,2011, 39(5):62-65.YANG C K, HUA Y M, HUA T. Insulation mechanism and application of insulation fiber material[J]. Cotton Textile Technology, 2011, 39(5):62-65.(in Chinese)
[9]ZHANG X S, WANG B, WU N, et al. Micro-nano ceramic fibers for high temperature thermal insulation[J]. Journal of Inorganic Materials, 2021, 36(3):245.
[10]LIAO D G, WANG Y N, XIE P Y, et al. A resilient and lightweight cellulose/graphene oxide/polymer-derived multifunctional carbon aerogel generated from Pickering emulsion toward a wearable pressure sensor[J]. Journal of Colloid and Interface Science, 2022, 628:574-587.
[11]PENG Y, XIE Y S, WANG L, et al. High-temperature flexible, strength and hydrophobic YSZ/SiO2nanofibrous membranes with excellent thermal insulation[J]. Journal of the European Ceramic Society, 2021, 41(2):1471-1480.
[12]GLYMOND D, VICK M J, GIULIANI F, et al. High-temperature fracture toughness of mullite with monoclinic zirconia[J]. Journal of the American Ceramic Society, 2017,100(4):1570-1577.
[13]焦秀玲,陈代荣.氧化铝基陶瓷连续纤维研究进展[J].硅酸盐学报,2024, 52(8):2738-2754.JIAO X L, CHEN D R. Progress on alumina ceramic continuous fibers[J]. Journal of the Chinese Ceramic Society,2024, 52(8):2738-2754.(in Chinese)
[14]曾佳琪,赵丽,唐海洲,等.氧化铝纤维的制备及其应用研究现状[J].合成纤维工业,2021, 44(5):65-70.ZENG J Q, ZHAO L, TANG H Z, et al. Research status of preparation and application of alumina fiber[J]. China Synthetic Fiber Industry, 2021, 44(5):65-70.(in Chinese)
[15]ZHANG P P, LU W J, WANG Y F, et al. Fabrication of flexible and amphiphobic alumina mats by electrospinning[J]. Journal of Sol-Gel Science and Technology, 2016, 80(3):690-696.
[16]仇小晗,李泳材,许梦月,等.静电纺陶瓷纳米纤维高温隔热材料的研究进展[J].合成纤维工业,2024, 47(4):62-67.QIU X H, LI Y C, XU M Y, et al. Research progress in high-temperature insulation materials of electrospun ceramic nanofiber[J]. China Synthetic Fiber Industry, 2024,47(4):62-67.(in Chinese)
[17]ESFAHANI H, JOSE R, RAMAKRISHNA S. Electrospun ceramic nanofiber mats today:synthesis, properties, and applications[J]. Materials, 2017, 10(11):1238.
[18]WEI M Y, XU J, YANG R W, et al. Synthesis of ultrafine rare-earth-zirconate high-entropy ceramic fibers via electrospinning[J]. Journal of the American Ceramic Society, 2022, 105(6):4449-4456.
[19]ZHAO B Y, HUANG H M, CHEN Q J. Fabrication and characterization of Y2Si2O7fibers prepared by electrospinning[J]. Journal of Non-Crystalline Solids, 2022, 594:121809.
[20]SHI F Y, HUANG S Y, WANG J W, et al. Multicomponent Si-Zr-based lightweight nanofiber films with a hollow structure exhibiting excellent thermal insulation properties[J]. Ceramics International, 2024, 50(2):3471-3479.
[21]MAHAPATRA A, MISHRA B G, HOTA G. Synthesis of ultra-fine α-Al2O3fibers via electrospinning method[J]. Ceramics International, 2011, 37(7):2329-2333.
[22]LIU P C, ZHU Y Z, MA J H, et al. Preparation of continuous porous alumina nanofibers with hollow structure by single capillary electrospinning[J]. Colloids and Surfaces A:Physicochemical and Engineering Aspects, 2013, 436:489-494.
[23]WANG Y, LI W, JIAO X L, et al. Electrospinning preparation and adsorption properties of mesoporous alumina fibers[J]. Journal of Materials Chemistry A, 2013, 1(36):10720-10726.
[24]WANG N, XIE Y S, LÜJ N, et al. Preparation of ultrafine flexible alumina fiber for heat insulation by the electrospinning method[J]. Ceramics International , 2022, 48(13):19460-19466.
[25]SU J H, LIU Y, PENG X J, et al. Preparation of α-Al2O3by low-temperature calcining γ-Al2O3with α-phase seed in-situ obtained by ball milling[J]. Materials Today Communications, 2023, 36:106681.
[26]ZHANG P P, CHEN D R, JIAO X L. Fabrication of flexible α-alumina fibers composed of nanosheets[J]. European Journal of Inorganic Chemistry, 2012, 2012(26):4167-4173.
基本信息:
DOI:10.12194/j.ntu.20251014001
中图分类号:TB383.2
引用信息:
[1]张梦娇,李文哲,王文强,等.柔性氧化铝基纳米纤维膜的制备及结构调控研究[J].南通大学学报(自然科学版),2026,25(01):48-55.DOI:10.12194/j.ntu.20251014001.
基金信息:
国家自然科学基金青年科学基金项目(52003126); 江苏省研究生科研与实践创新计划项目(KYCX24_3533)
2025-10-14
2025
2025-12-12
2025-12-08
2025
1
2026-01-14
2026-01-14
2026-01-14