碳纤维-碳纳米管多尺度增强聚四氟乙烯复合材料摩擦学性能研究

汤皓; 徐颖; 程先华

碳纤维-碳纳米管多尺度增强聚四氟乙烯复合材料摩擦学性能研究

汤皓¹,
徐颖^{1, 2},
程先华^1, ,

1.
上海交通大学　机械与动力工程学院, 上海 200240
2.
上海师范大学　信息与机电工程学院, 上海 201418

基金项目: 国家自然科学基金 (51975359)

详细信息

通讯作者:
程先华，博士，教授，博士生导师，研究方向为纳米表面工程及摩擦学　 E-mail: xhcheng@sjtu.edu.cn

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2022-01-14
- 修回日期: 2022-03-03
- 录用日期: 2022-03-19
- 网络出版日期: 2022-04-09

Tribological performance study of carbon fibre-carbon nanotube multiscale reinforced polytetrafluoroethylene composites

Hao TANG¹,
Ying XU^{1, 2},
Xianhua CHENG^{1
, ,}

1.
School of Mechanical Engineering, Shanghai Jiao Tong University, Shanghai 200240, China
2.
College of Information, Mechanical and Electronic Engineering, Shanghai Normal University, Shanghai 201418, China

摘要

摘要: 针对传统化学法易损伤纤维、污染严重的缺点，采用稀土LaCl₃表面处理方法合成碳纤维(Carbon Fibre, CF)-碳纳米管(Carbon Nanotube, CNT)微纳多尺度增强体，通过烧结工艺制备CF-CNT多尺度增强聚四氟乙烯(Polytetrafluoroethylene, PTFE)基复合材料。对增强体形貌、表面微晶结构以及复合材料硬度、晶体结构、浸润性等进行了表征，揭示了CF-CNT多尺度增强体对PTFE基复合材料结晶度、表面能的影响机制，在不同往复摩擦学试验参数下测试了复合材料的摩擦系数与磨损率，对摩擦过程各个阶段进行细致分析并提出了相应的摩擦磨损机制，结果表明：稀土LaCl₃表面处理方法相对传统方法具有不损伤纤维、无毒害的工艺优势；多尺度增强PTFE基复合材料磨损率降低了75.3%，优于同类研究；CF-CNT多尺度增强复合材料较小的表面能降低了起始摩擦系数；多尺度结构及La(III)提高了CF-CNT增强体与PTFE基体的界面结合性能，使材料在摩擦过程中不易产生大块硬质磨粒，并形成强度与稳定性较高的转移膜；复合材料摩擦学行为受往复频率及载荷影响显著，而且在高往复频率及低载荷下磨损率较低。本研究采用稀土LaCl₃表面处理方法合成CF-CNT多尺度增强体并将其用于提高聚四氟乙烯复合材料摩擦学性能，所得结论为高性能树脂基复合材料的设计提供了参考。
- LaCl₃ /
- 碳纤维 /
- 碳纳米管 /
- 聚四氟乙烯 /
- 往复摩擦学试验
Abstract: To avoid the fibre damage and serious pollution caused by the traditional chemical methods, this study synthesized the carbon fibre (CF)-carbon nanotube (CNT) micro-nano multiscale reinforcer by rare-earth LaCl₃ surface treatment method, and then prepared CF-CNT multiscale reinforced polytetrafluoroethylene (PTFE) composites via sintering process. The morphology and surface microcrystalline structure of the reinforcer, and the hardness, crystal structure and wettability of the composite were characterized, and the influence mechanism of the CF-CNT multiscale reinforcer on the crystallinity and surface energy of the PTFE composite was revealed. The coefficient of friction and wear rate of the composites were tested under different reciprocating tribological test parameters, every stage of the friction process was thoroughly discussed with the proposition of corresponding friction and wear mechanism. These results demonstrate that: the avoidance of fibre damage and toxic raw materials distinguishes the proposed CF-CNT reinforcer synthesis method from the traditional methods. The lower surface energy of CF-CNT reinforced composite decreases its initial friction coefficient. The wear rate of the CF-CNT reinforced composite is reduced by 75.3%, which is superior to the counterpart in similar studies. The multiscale structure and La(III) on CF-CNT improve the interface bonding performance of the CF-CNT reinforced composites, prevent the generation of large and hard wear debris during the surface yielding process as well as promoting the formation of high strength and stable transfer film. The tribological behaviors of the CF-CNT reinforced composites is sensitive to the reciprocating frequency and load, the higher frequency and lower load favour the lower wear rate. This study synthesized CF-CNT multiscale reinforcer via rare-earth LaCl₃ surface treatment method to enhance the tribological properties of PTFE composite, the obtained research conclusions are instructive for the design of high-performance polymer composite.
- LaCl₃ /
- carbon fibre /
- carbon nanotube /
- polytetrafluoroethylene /
- reciprocating tribological test

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图 1 超声30 min所得浓度为1.0 g/L的分散系静置不同时刻的沉降结果对比图：碳纳米管(CNT)-乙醇分散系静置1 h (a)及24 h (b)，RCNT-乙醇分散系静置1 h (c)及24 h (d)

Figure 1. Comparison of the sedimentation results of the dispersion system with a concentration of 1.0 g/L obtained by ultrasonicating for 30 min at different times: Carbon nanotube (CNT)-ethanol dispersion system kept still for 1 h (a) and 24 h (b), RCNT-ethanol dispersion system kept still for 1 h (c) and 24 h (d)

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图 2 (a, b) RCF-RCNT多尺度增强体形貌；(c) CF、RCF、RCF-RCNT的拉曼光谱

Figure 2. (a, b) Morphology of RCF-RCNT multiscale reinforcer; (c) Raman spectra of CF, RCF and RCF-RCNT.

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图 3 不同复合材料的X射线衍射光谱及结晶度$ {X}_{\mathrm{c}} $(a)及2θ=16° (b),18.14° (c)处的放大图

Figure 3. XRD pattern and crystallinity $ {X}_{\mathrm{c}} $ of different composites (a) and enlarged view at 2θ=16° (b) and 18.14° (c)

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图 4 不同复合材料的表面能

Figure 4. Surface energy of different composites

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图 5 不同复合材料的摩擦系数实时变化曲线图：(a) 2 min前(放大图)；(b) 2 min后(往复频率6 Hz，载荷16 N)

Figure 5. Real-time coefficient of friction curve of different composites: (a) magnified view before 2 min; (b) after 2 min (reciprocating frequency: 6 Hz, load: 16 N)

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图 6 不同复合材料的摩擦系数及磨损率

Figure 6. Coefficient of friction and wear rate of different composites

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图 7 复合材料磨损面典型形貌：(a~c) PTFE, (d~f) CF/PTFE, (g~i) RCF/PTFE, (j~l) CF-CNT/PTFE, (m~o) RCF-RCNT/PTFE

Figure 7. Typical worn surface morphology of composites: (a~c) PTFE, (d~f) CF/PTFE, (g~i) RCF/PTFE, (j~l) CF-CNT/PTFE, (m~o) RCF-RCNT/PTFE

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图 8 复合材料对磨球典型表面形貌：(a) PTFE, (b) CF/PTFE, (c) RCF/PTFE, (d) CF-CNT/PTFE, (e) RCF-RCNT/PTFE

Figure 8. Typical GCr15 ball surface morphology of (a) PTFE, (b) CF/PTFE, (c) RCF/PTFE, (d) CF-CNT/PTFE, (e) RCF-RCNT/PTFE after tribological test

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图 9 不同复合材料摩擦过程各阶段及其摩擦磨损机制简图

Figure 9. Diagram of the proposed friction and wear stage and corresponding mechanism of different composites

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图 10 复合材料磨粒脱落过程简图：(a) CF/PTFE, (b) CF-CNT/PTFE, (c) RCF/PTFE, (d) RCF-RCNT/PTFE

Figure 10. Schematic illustration of the wear debris generation process of CF/PTFE (a), CF-CNT/PTFE (b), RCF/PTFE (c), RCF-RCNT/PTFE (d) composites

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图 11 不同载荷下的RCF-RCNT/PTFE复合材料摩擦系数、摩擦力、磨损率及磨损量

Figure 11. Coefficient of friction, frictional force, wear rate and wear loss of RCF-RCNT/PTFE composites under different load

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图 12 不同往复频率下的RCF-RCNT/PTFE复合材料摩擦系数、磨损率及磨损量

Figure 12. Coefficient of friction, wear rate and wear loss of RCF-RCNT/PTFE composites under different reciprocating frequency

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图 13 往复频率为6 Hz (a)、10 Hz (b)，载荷为16 N时RCF-RCNT/PTFE复合材料摩擦学试验中的GCr15对磨球典型形貌

Figure 13. Typical worn surface morphology of GCr15 grinding ball after the tribological test of RCF-RCNT/Ep under 16 N and 6 Hz (a), 10 Hz (b)

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表 1 不同复合材料的硬度

Table 1. Hardness of different composites

Sample	Hardness (Shore D)
PTFE	57.0±2.9
CF/PTFE	61.7±1.5
RCF/PTFE	62.3±0.6
CF-CNT/PTFE	61.3±1.4
RCF-RCNT/PTFE	62.7±0.2

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表 2 不同复合材料的接触角

Table 2. Contact angle of different composites

Sample	Contact angle/(°)
Sample	Water	Diiodomethane
PTFE	109.0±4.4	78.1±5.9
CF/PTFE	120.8±0.5	76.4±1.8
RCF/PTFE	118.4±2.9	79.0±1.3
CF-CNT/PTFE	119.1±2.5	75.8±2.1
RCF-RCNT/PTFE	110.2±4.4	78.4±0.6

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表 3 所用液相的表面能

Table 3. Surface tension of the used test liquid

Wetting liquids	Surface tension $ {\gamma }_{l} $/(mJ·m⁻²)	Dispersion component $ {\gamma }_{l}^{d} $/(mJ·m⁻²)	Polar component $ {\gamma }_{l}^{p} $/(mJ·m⁻²)
Water	72.8	21.8	51.0
Diiodomethane	50.8	48.5	2.3

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表 4 相关研究中PTFE基复合材料摩擦学性能对比

Table 4. Tribological performance comparison of PTFE based composites in similar studies

Ref.	Composites	Type of friction	Test conditions	Wear rate / (×10⁻⁶ mm³·N⁻¹·m⁻¹)	Decrement of wear rate/%
[41]	PTFE	Reciprocating sliding	Counterface: φ=10 mm steel ball, load: 10 N, frequency: 10 Hz	304.8	−48.1
[41]	30vol.% h-BN/AO/PTFE	Reciprocating sliding		158.2	−48.1
[42]	PTFE/AP	Reciprocating sliding	Counterface: φ=9 mm Si₃N₄ ball, load: 10 N, frequency: 1 Hz	3.2	−44.1
[42]	6wt.% modified CF/PTFE/AP	Reciprocating sliding	Counterface: φ=9 mm Si₃N₄ ball, load: 10 N, frequency: 1 Hz	1.79	−44.1
[43]	PTFE	Reciprocating sliding	Counterface: φ=5 mm Si₃N₄ ball, load: 3 N, frequency: 2 Hz	2.5	−44.0
[43]	5wt.% CF/5wt.%BP/PTFE	Reciprocating sliding	Counterface: φ=5 mm Si₃N₄ ball, load: 3 N, frequency: 2 Hz	1.4	−44.0
[2]	PTFE	Continuous sliding	Counterface: φ=6 mm steel ball, load: 10 N, rotational speed: 200 r/min	390	−29.7
[2]	20wt.%CF/PTFE	Continuous sliding		274	−29.7
[1]	PTFE	Reciprocating sliding	Counterface: 5×5×25 mm steel pin, load: 50 N, frequency: 2 Hz	0.21	—
	15wt.% AF/PTFE			0.23	+9.5
	15wt.% CF/PTFE			0.24	+14.3
	15wt.% GF/PTFE			0.18	−14.3
	0.5wt.% BF/PTFE			0.15	−28.6
	0.5wt.% BF+ 10wt.%MoS₂/PTFE			0.17	−19.1
[20]	PI	Reciprocating sliding	Counterface: φ=4 mm steel ball, load: 4.5 N, velocity: 0.083 m/s	6.44	−72.2
[20]	5wt.% CF-CNT reinforcer/PI	Reciprocating sliding		1.79	−72.2
This study	PTFE	Reciprocating sliding	Counterface: φ=6 mm steel ball, load: 16 N, frequency: 6 Hz	321.6	−75.4
This study	5wt.% RCF-RCNT reinforcer/PTFE	Reciprocating sliding	Counterface: φ=6 mm steel ball, load: 16 N, frequency: 6 Hz	79.0	−75.4
Notes: h-BN—hexagonal boron nitride; AO—alumina particles; AP—aluminum dihydrogen phosphate; BP—black phosphorus; AF—aramid fiber; GF—glass fiber; BF—basalt fiber; PI—polyimide.

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