Preparation and Atomic Oxygen-Resistant Properties of Quaternary Ammonium Salt Modified Polyhedral Oligomeric Silsesquioxane/Polyimide Composite Fibers

doi:10.19894/j.issn.1000-0518.250292

Chinese Journal of Applied Chemistry ›› 2026, Vol. 43 ›› Issue (1): 31-40.DOI: 10.19894/j.issn.1000-0518.250292

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Preparation and Atomic Oxygen-Resistant Properties of Quaternary Ammonium Salt Modified Polyhedral Oligomeric Silsesquioxane/Polyimide Composite Fibers

Fang-Fang LIU¹, Hai-Bo YAO¹, Guo-Min LI¹, Li-Peng WANG², Zhi-Xin DONG¹(), Xue-Peng QIU¹()

^1.CAS Key Laboratory of High-performance Synthetic Rubber and Its Composite Materials，Changchun Institute of Applied Chemistry，Chinese Academy of Sciences，Changchun 130022，China
^2.Xi'an Institute of Space Radio Technology，Xi'an 710100，China

Received:2025-07-22 Accepted:2025-10-30 Published:2026-01-01 Online:2026-01-26
Contact: Zhi-Xin DONG,Xue-Peng QIU
About author:xp_q@ciac.ac.cn
zxdong@ciac.ac.cn；
Supported by:
the National Key Research and Development Program of China(2023YFB3811901);the Key Program of the Chinese Academy of Sciences(ZDBS-ZRKJZ-TLC020);the Youth Innovation Promotion Association of CAS(Y2023064);Jilin Province Outstanding Young Scientist Program(20230508113RC);the Science and Technology Program of Tianjin(23YFYSHZ00230);Jilin Province Youth Development Project(20240602121RC)

Abstract

Abstract:

Herein， polyhedral oligomeric silsesquioxane （POSS） nanoparticles were modified by quaternary ammonium， followed by adding into polyamic acid （PAA） spinning solution. Then series of QA-POSS/PI composite fibers were afforded via wet-spinning process. The as-prepared composite fibers showed good thermal properties with 5% thermal decomposition temperature（T_5%） and glass transition temperature （T_g） values of 558 ℃ and 395 ℃. Based on X-ray photoelectron spectroscopy （XPS） and inductively coupled plasma （ICP） measurement results， the silicon contents on fiber surface were higher than those in total fiber， which indicated that silicon showed gradient distribution in composite fibers. When additive amount of QA-POSS nanoparticles was raised from 0% to 15%， the surface topographies of composite fibers displayed a clear change from roughness to compact， and mass loss decreased obviously from 1.40 mg/cm² to 0.10 mg/cm² after AO erosion with the fluence of 3.17×10²⁰ atoms/cm². Actually， the lowest loss of mechanical properties was seen for the composite fibers when 5% QA-POSS particles were added. Fracture strength and initial modulus retentions of the fibers were 89.36% and 89.35%， respectively. And the corresponding decay rate of the strength was seen as 1.58×10^-13 Pa·cm²/atom.

Key words: Polyimide fibers, Polyhedral oligomeric silsesquioxanes, Anti-atomic oxygen

CLC Number:

O631

Fang-Fang LIU, Hai-Bo YAO, Guo-Min LI, Li-Peng WANG, Zhi-Xin DONG, Xue-Peng QIU. Preparation and Atomic Oxygen-Resistant Properties of Quaternary Ammonium Salt Modified Polyhedral Oligomeric Silsesquioxane/Polyimide Composite Fibers[J]. Chinese Journal of Applied Chemistry, 2026, 43(1): 31-40.

Figures/Tables 10

Fig.1 Preparation process of spinning solution and composite fibers

Fig.2 FT-IR spectra of blank PI fiber and QA-POSS/PI composite fibers

Table 1 Theoretical and test results of silicon content in the composite fibers

Sample	w（QA-POSS）/% in PAA	Calculated w（silicon）/%	w（silicon）/% measured by XPS	w（silicon）/% measured by ICP
1	2.5	0.50	1.75	0.65
2	5.0	1.00	2.35	0.71
3	7.5	1.50	2.92	1.23
4	10.0	2.00	3.18	1.69
5	15.0	3.00	5.99	2.73

Fig.3 Cross-sectional morphology images of composite fibers with QA-POSS additions of 2.5% （A1， A2）， 5% （B1， B2）， and 10% （C1， C2）. Quantitative analysis of Si element content in the central regions （A1， B1， C1） and edge regions （A2， B2， C2） of the fibers

Fig.4 TGA and DMA curves of blank PI fiber and QA-POSS/PI composite fibers

Fig.5 Mass loss of Kapton and composite films after AO erosion

Fig.6 Surface morphologies of （A0-A3） blank PI fiber， composite fibers with （B0-B3） 2.5% QA-POSS，（C0-C3） 5% QA-POSS，（D0-D3） 7.5% QA-POSS，（E0-E3） 10% QA-POSS， and （F0-F3） 15% QA-POSS additive amount before and after AO erosion

Fig.7 XPS spectra of composite fibers with 5% and 15% QA-POSS additive amount before and after AO erosion

Table 3 Surface elemental content of the composite fibers before and after exposure to AO

Element type	Surface elemental mass fraction by XPS/%
	Composite fibers with 5% QA-POSS additive amount		Composite fibers with 15% QA-POSS additive amount
	Before AO exposure	After AO exposure	Before AO exposure	After AO exposure
C	77.68	39.04	75.27	20.37
O	15.93	38.62	15.64	50.71
Si	2.35	20.57	5.99	27.82

Fig.8 Variation on （A） strength，（B） modulus and （C） strength decay rate of composite fibers before and after AO erosion

References 29

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Preparation and Atomic Oxygen-Resistant Properties of Quaternary Ammonium Salt Modified Polyhedral Oligomeric Silsesquioxane/Polyimide Composite Fibers

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