Journal of Textile Research ›› 2026, Vol. 47 ›› Issue (04): 71-79.doi: 10.13475/j.fzxb.20250804401

• Fiber Materials • Previous Articles     Next Articles

Preparation of ultra-high temperature resistant Al2O3-based ceramic fibers and their forming mechanism

LI Shouzhen1,2, ZHA Tiantian3, ZHOU Weitao3, SI Yang4()   

  1. 1 College of Materials Science and Engineering, Qingdao University, Qingdao, Shandong 266071, China
    2 College of Art and Design, Nantong Vocational University, Nantong, Jiangsu 226007, China
    3 Research Institute of Textile and Clothing Industries, Zhongyuan University of Technology, Zhengzhou, Henan 450007, China
    4 Innovation Center for Textile Science and Technology, Donghua University, Shanghai 201620, China
  • Received:2025-08-20 Revised:2026-01-15 Online:2026-04-15 Published:2026-06-24
  • Contact: SI Yang E-mail:yangsi@dhu.edu.cn

Abstract:

Objective Ceramic fibrous materials have the advantages of high temperature resistance, high strength, and excellent oxidation resistance, with wide applications in aerospace, new energy vehicles, oil-water separation and other fields. Due to the sudden increase in grain size and defects in Al2O3-based fibers materials at ultra-high temperatures, the brittleness of the fibers limited their use in extreme environments. In this research, ZrO2 is used as an inhibitor of Al2O3 crystal growth to slow down the crystal growth rate, aiming at the preparation of ultra-high temperature resistant Al2O3-based fibers through centrifugal spinning and calcination, providing new method for the development of ceramic fibers.

Method Al2O3 precursor sols were prepared by sol-gel technology and Al2O3 precursor gel fibers were prepared by centrifugal spinning, and the viscosity of spinning solution was adjusted by adding polymer. Clear and transparent Al2O3 precursor sols were prepared from organic Al salt, Al strong acid salt and solvent water, and then the formation mechanism of Al2O3-based fibers were studied. The Al2O3 gel fibers were obtained by drawing spinning solution using centrifugal force. The influence of spinning solutions on gel fibers and calcined fibers were analysed, indicating that the higher spinning solution temperature led to the better temperature resistance of the obtained fiber.

Results Al2O3-based fibers were fabricated by sol-gel centrifugal spinning and calcination method, First, the formation mechanism of Al precursor sols was studied, with water playing the role of solvent, AIP and AlCl3·6H2O as the Al sources, CH2O7Zr2 as the Zr sources, PVP as the polymer to regulate the spinning solution viscosity. AIP was dissolved in aluminum chloride aqueous solution to form a homogeneous system, which avoids the application of organic solvents and reduces the production cost and reduces the pollution to the external environment. Then, the forming mechanism of Al2O3-based fibers, influence of spinning solution temperature on gel fibers and Al2O3-based fibers were discussed. The spinning fluid of Al2O3 precursor was thrown out fast by centrifugal force and rapidly formed in air. Al2O3 and ZrO2 precursor colloidal particles were rapidly hydrolyzed and condensed to form precursor sol fibers. The organic components in precursor gel fibers were removed by calcination to obtain Al2O3-based fibers. After calcination, the average diameter of gel fiber was reduced to as low as 1.88 μm. The changes in the crystal structure of Al2O3 during the calcination process were monitored using XRD, and the Al2O3-based fibers exhibited an amorphous microstructure below 1 000 ℃. The spinning fluid temperature was inversely proportional to the diameter, showing that the higher the temperature the smaller the diameter of gel fiber. The temperature of the spinning solution affected the particle composition of the fibers. It was found that higher temperature of the spinning fluid resulted in smaller particles that formed the fibers.

Conclusion Al2O3-based fibers were fabricated by sol-gel method combined with centrifugal spinning and calcination technology, and the spinning fluid temperature and calcination temperature were optimized to prepare Al2O3-based fibers materials with smooth surface and fine grain size. The average diameter of the Al2O3-based fibers samples prepared was as low as 1.88 μm, indicating that Al2O3-based fibers were successfully prepared, and the fiber diameter was adjustable in the range of 1.88-20.40 μm. The Al2O3-based fibers exhibited excellent high temperature resistance. When the calcination temperature reached 1 300 ℃, the particles that formed the fibers were very small and could be used as thermal protection materials in aerospace, high-temperature filtration, and other fields.

Key words: inorganic fiber, ceramic fiber, Al2O3-based fiber, ultra-high temperature resistance, crystal structure, spinning temperature

CLC Number: 

  • TQ343.5

Fig.1

Preparation process of Al2O3-based fiber"

Fig.2

Morphology of Al2O3-based fibers. (a) Al2O3-based fibers; (b) Cross-section"

Fig.3

SEM images and EDS mapping of Al2O3-based fibers. (a) Al2O3-based fibers SEM image; (b) Al element; (c) Zr element; (d) O element"

Fig.4

TG curves of Al2O3 precursor gel fibers"

Fig.5

Effects of calcination temperature on crystalline structure of Al2O3-based fibers"

Fig.6

Effects of spinning solution temperature on morphology of gel fibers"

Fig.7

Fiber diameter distribution at different spinning solution temperatures"

Fig.8

Effects of spinning solution temperature on morphology of fibers after calcination at 1 000 ℃"

Fig.9

Diameter distribution of calcined fibers at different spinning solution temperatures (calcination temperature of 1 000 ℃)"

Fig.10

Effects of spinning solution temperature on morphology after calcination (calcination temperature of 1 300 ℃)"

[1] 徐汇, 张培垣, 徐娜娜, 等. 耐高温SiO2/ZrO2纳米纤维膜的力学和隔热性能[J]. 材料研究学报, 2024, 38(5): 365-372.
doi: 10.11901/1005.3093.2023.232
XU Hui, ZHANG Peiyuan, XU Nana, et al. Mechanical property and thermal insulation performance of SiO2/ZrO2 nanofiber membranes with high thermal stability[J]. Chinese Journal of Materials Research, 2024, 38(5): 365-372.
doi: 10.11901/1005.3093.2023.232
[2] 孙敬伟, 王洪磊, 杨蕊, 等. 热处理环境对Al2O3纤维力学性能及微观结构的影响[J]. 材料工程, 2023, 51(8): 110-119.
doi: 10.11868/j.issn.1001-4381.2023.000146
SUN Jingwei, WANG Honglei, YANG Rui, et al. Effect of heat treatment environment on mechanical properties and microstructure of alumina fibers[J]. Journal of Materials Engineering, 2023, 51(8): 110-119.
doi: 10.11868/j.issn.1001-4381.2023.000146
[3] WANG H X, CHENG L D, YU J Y, et al. Biomimetic Bouligand chiral fibers array enables strong and superelastic ceramic aerogels[J]. Nature Communications, 2024, 15: 336.
doi: 10.1038/s41467-023-44657-2 pmid: 38184664
[4] LI L, ZHOU Y Q, GAO Y, et al. Large-scale assembly of isotropic nanofiber aerogels based on columnar-equiaxed crystal transition[J]. Nature Communications, 2023, 14: 5410.
doi: 10.1038/s41467-023-41087-y pmid: 37670012
[5] 罗萌, 向阳, 彭志航, 等. 纤维多孔陶瓷的研究进展[J]. 材料工程, 2022, 50(11): 63-72.
doi: 10.11868/j.issn.1001-4381.2021.000742
LUO Meng, XIANG Yang, PENG Zhihang, et al. Research progress of fibrous porous ceramic[J]. Journal of Materials Engineering, 2022, 50(11): 63-72.
doi: 10.11868/j.issn.1001-4381.2021.000742
[6] 高晨光, 孙晓亮, 陈君, 等. 基于湿法纺丝技术的SiBCN-rGO陶瓷纤维的组织结构、力学和吸波性能[J]. 无机材料学报, 2025, 40(3): 290-296.
GAO Chenguang, SUN Xiaoliang, CHEN Jun, et al. SiBCN-rGO ceramic fibers based on wet spinning technology: microstructure, mechanical and microwave-absorbing properties[J]. Journal of Inorganic Materials, 2025, 40(3): 290-296.
doi: 10.15541/jim20240391
[7] LI L, JIA C, LIU Y, et al. Nanograin-glass dual-phasic, elasto-flexible, fatigue-tolerant, and heat-insulating ceramic sponges at large scales[J]. Materials Today, 2022, 54: 72-82.
doi: 10.1016/j.mattod.2022.02.007
[8] YUAN L, LIU Z L, TIAN C, et al. Synthesis and characterization of mullite-ZrO2 porous fibrous ceramic for highly efficient oil-water separation[J]. Ceramics International, 2021, 47(16): 22709-22716.
doi: 10.1016/j.ceramint.2021.04.286
[9] LI X L, QIU R X, SUN Y X, et al. Study on the preparation and properties of zirconium ceramic fiber toughened composite lightweight alkali-activated slag-based high performance thermal insulation material[J]. Construction and Building Materials, 2025, 484: 141875.
doi: 10.1016/j.conbuildmat.2025.141875
[10] DAI J, WU F, LIU H L, et al. Achieving robust α-alumina nanofibers by ligand confinement coupled with local disorder tuning[J]. ACS Nano, 2024, 18(52): 35418-35428.
doi: 10.1021/acsnano.4c12568 pmid: 39688462
[11] 崔婧妍, 魏英, 尹洪峰, 等. 静电纺丝法制备微纳含硼SiC纤维及其电磁波吸收性能[J]. 复合材料学报, 2026, 43(1): 268-280.
CUI Jingyan, WEI Ying, YIN Hongfeng, et al. Fabrication of micro-nano boron-containing SiC fibers by electrospinning and its electromagnetic wave absorption properties[J]. Acta Materiae Compositae Sinica, 2026, 43(1): 268-280.
[12] XU L, RAN P, ZHOU W Q, et al. All-inorganic metafabric scintillators for conformally flexible and wearable X-ray detection and imaging[J]. Science Advances, 2025, 11(26): eadv5537.
[13] LIU H L, HUO X D, ZHAO P L, et al. Confined gelation synthesis of flexible barium aluminate nanofibers as a high-performance refractory material[J]. ACS Nano, 2024, 18(42): 29273-29281.
doi: 10.1021/acsnano.4c11854 pmid: 39377726
[14] 贾玉娜, 曹旭, 焦秀玲, 等. 无机酸铝体系氧化铝连续纤维的制备技术研究[J]. 无机材料学报, 2023, 38(11): 1257-1264.
JIA Yuna, CAO Xu, JIAO Xiuling, et al. Preparation of alumina ceramic continuous fibers with inorganic acidic aluminum sol as precursor[J]. Journal of Inorganic Materials, 2023, 38(11): 1257-1264.
doi: 10.15541/jim20230153
[15] DAI C H, ZHANG Z H, WANG T C. Preparation and heat-insulating properties of Al2O3-ZrO2(Y2O3) hollow fibers derived from cogon using an orthogonal experimental design[J]. RSC Advances, 2019, 9(20): 11305-11311.
doi: 10.1039/C9RA01176E
[16] SU L, WANG H J, JIA S H, et al. Highly stretchable, crack-insensitive and compressible ceramic aerogel[J]. ACS Nano, 2021, 15(11): 18354-18362.
doi: 10.1021/acsnano.1c07755 pmid: 34766747
[17] LI Z W, CUI Z W, ZHAO L H, et al. High-throughput production of kilogram-scale nanofibers by Kármán vortex solution blow spinning[J]. Science Advances, 2022, 8(11): eabn3690.
[18] 陈博文, 王敬晓, 姜佑霖, 等. 基于离心纺丝技术制备稳定的碳化锆纤维[J]. 无机材料学报, 2020, 35(12): 1385-1390.
doi: 10.15541/jim20200031
CHEN Bowen, WANG Jingxiao, JIANG Youlin, et al. Stable zirconium carbide fibers fabricated by centrifugal spinning technique[J]. Journal of Inorganic Materials, 2020, 35(12): 1385-1390.
doi: 10.15541/jim20200031
[19] XI C, LIU X Y, WANG T C, et al. Heat-insulating properties of hollow Al2O3-ZrO2(CeO2)fibers fabricated using pampas grass as the template[J]. Ceramics International, 2021, 47(2): 2000-2007.
doi: 10.1016/j.ceramint.2020.09.031
[20] GUO P F, SU L, PENG K, et al. Additive manufacturing of resilient SiC nanowire aerogels[J]. ACS Nano, 2022, 16(4): 6625-6633.
doi: 10.1021/acsnano.2c01039
[21] LI L, FANG B, REN D S, et al. Thermal-switchable, trifunctional ceramic-hydrogel nanocomposites enable full-lifecycle security in practical battery systems[J]. ACS Nano, 2022, 16(7): 10729-10741.
doi: 10.1021/acsnano.2c02557
[22] 吴红, 刘呈坤, 毛雪, 等. 柔性ZrO2纳米纤维膜的制备及其应用研究现状[J]. 纺织学报, 2020, 41(7): 167-173.
WU Hong, LIU Chengkun, MAO Xue, et al. Research progress in preparation and application of flexible zirconia nanofibers by electrospinning[J]. Journal of Textile Research, 2020, 41(7): 167-173.
doi: 10.1177/004051757104100213
[23] SHAO W L, YUE W L, REN L B, et al. Al2O3/SiO2 sponges with a three-dimensional lamellar structure based on solution blow spinning for superior thermal insulation and high temperature filtration[J]. Separation and Purification Technology, 2025, 376: 134088.
doi: 10.1016/j.seppur.2025.134088
[24] 范红娜, 许西庆, 李鑫, 等. 氧化铝改性硅基陶瓷型芯制备及结晶动力学[J]. 材料工程, 2024, 52(5): 212-217.
doi: 10.11868/j.issn.1001-4381.2022.001057
FAN Hongna, XU Xiqing, LI Xin, et al. Preparation and crystallization kinetics of silica-based ceramic cores modified by alumina[J]. Journal of Materials Engineering, 2024, 52(5): 212-217.
doi: 10.11868/j.issn.1001-4381.2022.001057
[25] 彭雨晴, 牟世伟, 韩克清, 等. 高性能SiBN(C)陶瓷纤维的热稳定性能及透波性能[J]. 复合材料学报, 2016, 33(2): 358-365.
PENG Yuqing, MOU Shiwei, HAN Keqing, et al. Thermal stability and wave permeability of high performance SiBN(C) ceramic fibers[J]. Acta Materiae Compositae Sinica, 2016, 33(2): 358-365.
[26] MA D H, LIU B X, JIN X T, et al. Rheologic behaviors and continuously dry spinning of polyacetylacetonatozirconium fibers[J]. Materials Letters, 2020, 258: 126824.
doi: 10.1016/j.matlet.2019.126824
[27] 陆瑶瑶, 叶俊涛, 阮承祥, 等. 二氧化钛/多孔碳纳米纤维复合材料的制备及其光催化性能[J]. 纺织学报, 2024, 45(4): 67-75.
LU Yaoyao, YE Juntao, RUAN Chengxiang, et al. Preparation and photocatalytic performance of titanium dioxide/porous carbon nanofibers composite material[J]. Journal of Textile Research, 2024, 45(4): 67-75.
doi: 10.1177/004051757504500112
[28] CALISIR M D, KILIC A. A comparative study on SiO2 nanofiber production via two novel non-electrospinning methods: centrifugal spinning vs solution blowing[J]. Materials Letters, 2020, 258: 126751.
doi: 10.1016/j.matlet.2019.126751
[29] XIA L, JU J G, XU W, et al. Preparation and characterization of hollow Fe2O3 ultra-fine fibers by centrifugal spinning[J]. Materials & Design, 2016, 96: 439-445.
[30] HROMÁDKO L, MOTOLA M, ČIČMANCOVÁ V, et al. Facile synthesis of WO3 fibers via centrifugal spinning as an efficient UV- and VIS-light-driven photocatalyst[J]. Ceramics International, 2021, 47(24): 35361-35365.
doi: 10.1016/j.ceramint.2021.09.079
[31] GUO J R, FU S B, DENG Y P, et al. Hypocrystalline ceramic aerogels for thermal insulation at extreme conditions[J]. Nature, 2022, 606(7916): 909-916.
doi: 10.1038/s41586-022-04784-0
[32] XU L, RAN P, ZHOU W Q, et al. All-inorganic metafabric scintillators for conformally flexible and wearable X-ray detection and imaging[J]. Science Advances, 2025, 11(26): eadv5537.
[33] GAO Y, YU P H, ZHANG J, et al. Compressible piezoelectric ceramic nanofiber aerogels with multifunction[J]. Advanced Fiber Materials, 2025, 7(3): 937-949.
doi: 10.1007/s42765-025-00535-8
[1] QI Mengyuan, XIAO Guowei, DU Jinmei, XU Changhai, YANG Hongying. Preparation and properties of waterborne polyurethane/nano silica modified basalt fiber fabrics [J]. Journal of Textile Research, 2026, 47(02): 172-180.
[2] SHI Zhicheng, CHEN Fengxiang, WANG Mengyun, BAI Jie, LI Juan, BAI Meng, FU Guangwei, XU Weilin. Current status and development trends of high-performance inorganic fibers and their products for aerospace and aeronautical applications [J]. Journal of Textile Research, 2025, 46(12): 233-242.
[3] WEI Peng, LI Zhiqiang, LI Jiaojiao, LI Junhui, LIU Dong, GENG Jiajun. Influence of solid-state polymerization on structure and properties of naphthalene ring structure aromatic liquid crystal copolyester [J]. Journal of Textile Research, 2024, 45(09): 50-55.
[4] YU Wen, DENG Nanping, TANG Xiangquan, KANG Weimin, CHENG Bowen. Review on preparation and applications of electro-blown spun micro-nano inorganic fibers [J]. Journal of Textile Research, 2024, 45(07): 230-239.
[5] YUAN Wei, YAO Yongbo, ZHANG Yumei, WANG Huaping. Alkaline enzyme treatment process for preparation of Lyocell cellulose pulp [J]. Journal of Textile Research, 2020, 41(07): 1-8.
[6] . Biodegradability of cellulose fibers [J]. Journal of Textile Research, 2015, 36(11): 20-26.
[7] LIANG Lie-feng;WENG Jie. Preparation of calcium phosphate ceramic fibers by using silk as carrier [J]. JOURNAL OF TEXTILE RESEARCH, 2005, 26(4): 14-16.
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
No Suggested Reading articles found!