High thermal stability Cu2O@OZrP micro-nano hybrids for melt-spun excellent antibacterial activity polyester fibers

doi:10.1016/j.jmst.2021.01.013

Abstract

Abstract:

Public safety incidents caused by bacterial infections have attracted widespread attention towards antibacterial textiles (fibers, fabrics, etc.). Nevertheless, it is still challenging to efficiently load inorganic nano-antibacterial materials in polymer fibers. In this work, zirconium phosphate (ZrP, layered micro-nano materials) was utilized as a micro-nano carrier. The octadecyl triphenyl phosphonium bromide (OTP) was intercalated between the ZrP sheets by the ion exchange method to improve the carrier-polymer compatibility and the antibacterial performance. Through in-situ chemical reduction, the ultra-small nano-sized cuprous oxide (Cu₂O < 5 nm) was loaded on the outer surface of ZrP to realize the uniform and stable dispersion of the Cu ₂O on the carrier and improve the antibacterial performance. The ZrP nanosheets loaded with Cu₂O and OTP (Cu₂O@OZrP) had excellent antibacterial properties, and the antibacterial rate against E. coli, S. aureus and C. albicans was more than 99 %. The intercalation amount of OTP in Cu₂O@OZrP can reach 16 %, and the thermal stability was excellent and a significant increase in the Zeta potential. Indeed, the decomposition temperature was greater than 350 °C, which was suitable for high-temperature melt processing of polymers. Consequently, we prepared PET/Cu₂O@OZrP fibers using polyethylene glycol terephthalate (PET), which accounts for 70 % of the total chemical fibers, as the fiber matrix. PET/Cu₂O@OZrP fibers exhibited excellent mechanical property and antibacterial performance when the content of Cu₂O@OZrP was only 0.2 %. The antibacterial rate against five types of bacteria including super bacteria (MRSA, VRE) was more than 99 %.

Key words: Cu₂O@OZrP, Hybrid material, OTP, Fibers, Antibacterial

Jialiang Zhou, Yaping Wang, Weinan Pan, Hengxue Xiang, Peng Li, Zhe Zhou, Meifang Zhu. High thermal stability Cu₂O@OZrP micro-nano hybrids for melt-spun excellent antibacterial activity polyester fibers[J]. J. Mater. Sci. Technol., 2021, 81: 58-66.

Figures/Tables 8

Fig. 1. SEM images of (a) neat α-ZrP, (b) OZrP, (c) Cu 2O@ZrP nanosheets; TEM images of (d) neat α-ZrP, (e) Cu 2O@OZrP nanosheets, (f) enlarged view of the red area in (e), (g) element mapping of the Cu2O@ZrP nanosheets.

Fig. 2. (a, b) XRD patterns of ZrP, Cu2O@ZrP and Cu2O@OZrP, (c) schematic illustration of the synthetic procedure of the Cu2O@OZrP nanosheets.

Fig. 3. (a) FTIR spectra and (b) TGA curves of ZrP, Cu2O@ZrP and Cu2O@OZrP, (c) digital photos of the dispersibility of ZrP, Cu2O@ZrP and Cu2O@OZrP in n-hexane and water.

Table 1 Antibacterial activity of Cu2O@OZrP nanosheets.

Microbes	Samples	Sample concentration (mg/L)	Viable bacterial colonies after 24 h contact (CFU/mL)	Microbial reduction (%)	MIC
E. coli	Blank	0	7.1 × 10 ⁶	No effect	>10,000
E. coli	Cu₂O@OZrP	25	<1	>99	25
S. aureus	Blank	0	1.1 × 10 ⁶	No effect	>10,000
S. aureus	Cu₂O@OZrP	25	<1	>99	25
C. albicans	Blank	0	8.3 × 10 ⁴	No effect	>10,000
C. albicans	Cu₂O@OZrP	25	<1	>99	25

Fig. 4. Representative fluorescence microscopy images of E. coli and S. aureus: (a, c) control, (b, d) treated with Cu2O@OZrP nanosheets for 6 h and subsequently stained briefly (30 min) with DCFH-DA (2,7-dichlorofuorescin diacetate). SEM images of E. coli cells treated by Cu2O@OZrP (e) 3 h, (g) 8 h, (f, h) enlarged view of the red area; TEM images of E. coli cells treated by Cu2O@OZrP (i) 3 h, (k) 8 h, (j, l) enlarged view of the red area.

Fig. 5. Cytotoxicity of ZrP, OZrP, Cu2O@OZrP on NIH3T3 (±SD,n = 3), the concentrations of the samples were set at 0.04, 0.2, 1, 5, 25, 100 and 500 mg/mL.

Fig. 6. Digital photos of fibers: (a) PET, (b) PET/Cu2O@OZrP-0.05 %, (c) PET/Cu2O@OZrP-0.1 %, (d) PET/Cu2O@OZrP-0.2 %, (e) PET/Cu2O@OZrP-0.4 %; SEM images of fibers: (f) PET/Cu2O@OZrP-0.05 %, (g) PET/Cu2O@OZrP-0.1 %, (h) PET/Cu2O@OZrP-0.2 %, (i) PET/Cu2O@OZrP-0.4 %; (j) mechanical performance of PET/Cu2O@ZrP fibers.

Table 2 Antibacterial activity of PET/Cu2O@OZrP fibers.

Microbes	Samples	Blank sample viable colonies (CFU/mL)	Viable colonies (CFU/mL)	Microbial reduction (%)
E. coli	PET	1.5 × 10 ⁶	1.5 × 10 ⁶	No effect
E. coli	PET/Cu₂O@OZrP-0.2%	1.5 × 10 ⁶	<1	>99
S. aureus	PET	8.3 × 10 ⁵	8.3 × 10 ⁵	No effect
S. aureus	PET/Cu₂O@OZrP-0.2%	8.3 × 10 ⁵	<1	>99
C. albicans	PET	6.1 × 10 ⁵	6.1 × 10 ⁵	No effect
C. albicans	PET/Cu₂O@OZrP-0.2%	9.6 × 10 ⁴	<1	>99
MRSA	PET	1.6 × 10 ⁶	1.6 × 10 ⁶	No effect
MRSA	PET/Cu₂O@OZrP-0.2%	1.6 × 10 ⁶	<1	>99
VRE	PET	2.1 × 10 ⁶	2.1 × 10 ⁶	No effect
VRE	PET/Cu₂O@OZrP-0.2%	2.1 × 10 ⁶	<1	>99

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High thermal stability Cu₂O@OZrP micro-nano hybrids for melt-spun excellent antibacterial activity polyester fibers

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