Research progress of preparation and tribological application of two-dimensional layered Ti3C2Tx
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摘要: 二维层状材料不仅具有极高的承载能力，并且凭借其超薄的厚度在摩擦过程能较容易地进入摩擦接触区。因此，它们在减少摩擦和磨损方面具有巨大的研究和应用潜力。Mxenes作为一种类似于石墨烯的二维层状材料，具有独特的结构和丰富的官能团，其中Ti3C2Tx Mxenes因低层间剪切阻力、高比表面积、良好的分散性等优点而被广泛用作润滑添加剂。本文主要介绍了二维层状Ti3C2Tx的主要制备方法，包括“自上而下”和“自下而上”两种制备路线。同时对二维Ti3C2Tx作为液体润滑剂添加剂、固体润滑涂层添加剂、复合材料增强相的摩擦学应用及效果进行综述，并对其润滑机制进行了探讨。进一步对二维Ti3C2Tx的制备技术的发展和其作为新型润滑材料的应用前景作出展望。Abstract: The two-dimensional layered material not only has a very high load bearing capacity, but also can easily enter the friction contact zone during the friction process by virtue of its ultra-thin thickness. Therefore, they have great research and application potential in reducing friction and wear. As a two-dimensional layered material similar to graphene, Mxenes has a unique structure and rich functional groups. Among them, Ti3C2Tx Mxenes is widely used as a lubricating additive because of its advantages such as shear resistance between low layers, high specific surface area and good dispersion. This paper mainly introduces the main preparation methods of two-dimensional layered Ti3C2Tx, including "top-down" and "bottom-up" preparation routes. The tribological applications and effects of 2D Ti3C2Tx as liquid lubricant additive, solid lubricant coating additive and composite reinforcement phase are reviewed, and the lubrication mechanism of Ti3C2Tx is discussed. Further, the development of 2D Ti3C2Tx preparation technology and its application as a new lubrication material are prospected.
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Key words:
- MXenes /
- two-dimensional Ti3C2Tx /
- lubricating additive /
- tribological property /
- lubrication mechanism
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图 2 (a) Ti3C2Tx的氢氟酸刻蚀法[22]；(b) 手风琴状多层Ti3C2Tx的SEM图像[22]；(c) 多层Ti3C2Tx的插层与剥离[24] ；(d) 四甲基氢氧化铵插层-剥离的Ti3C2Tx纳米片的SEM图像[25]
Figure 2. (a) Hydrofluoric acid etching of Ti3C2Tx[22]; (b) SEM image of accordion-like multilayer Ti3C2Tx[22]; (c) Intercalation and stripping of multilayer Ti3C2Tx[24]; (d) SEM image of Ti3C2Tx nanosheets obtained by efficient intercalation and stripping with tetramethylammonium hydroxide[25]
图 6 (a) TDPA-Ti3C2合成路线；(b) 纯蓖麻油、添加0.1wt%未改性Ti3C2Tx 和TDPA改性Ti3C2Tx的蓖麻油润滑下的摩擦系数随时间变化规律；(c) 各实验组对应的磨损率[42]
Figure 6. (a) Synthesis route of TDPA-Ti3C2; (b) Time variation of friction coefficient of lubrication with pure castor oil, castor oil with 0.1wt% unmodified Ti3C2Tx and castor oil with TDPA modified Ti3C2Tx; (c) Wear rate of each experimental group[42]
TDPA—Tetradecyl phosphonic acid
图 7 (a) 斜坡载荷作用下纯全氟聚醚(PFPE)、添加未改性Ti3C2Tx的PFPE和添加聚[2-(全氟辛基)甲基丙烯酸乙酯] (PPFMA)-g-Ti3C2Tx的PFPE润滑下的摩擦系数随时间变化规律；(b) 斜坡频率作用下各对应实验组的摩擦系数随时间变化规律[43]
Figure 7. (a) Time variation of friction coefficient of lubrication with pure PFPE, PFPE with unmodified Ti3C2Tx and PFPE with PPFMA-g-Ti3C2Tx under slope load; (b) Time variation of friction coefficient of each experimental group under slope frequency[43]
PPFMA—Poly[2-(perfluorooctyl)ethyl methacrylate)]; PFPE—Perfluoropolyether; COF—Coefficient of friction
图 9 (a) Si3N4与蓝宝石超润滑系统示意图；(b) 在Ti3C2Tx-甘油溶液润滑下Si3N4和蓝宝石表面的接触区示意图；((c)~(e)) 边界润滑接触区；(f) 弹性流体动力润滑示意图[48]
Figure 9. (a) Si3N4 and sapphire super lubrication system; (b) Diagram of contact zone between Si3N4 and sapphire surface lubricated by Ti3C2Tx-glycerin solution; ((c)-(e)) Boundary lubrication contact area; (f) Diagram of elastic hydrodynamic lubrication[48]
图 12 (a) MoS2/Ti3C2Tx复合涂层制备及摩擦试验示意图；(b) MoS2/Ti3C2Tx复合涂层与钢对钢、MoS2涂层对钢和Ti3C2Tx涂层对钢稳态摩擦系数；(c) MoS2/Ti3C2Tx复合涂层在不同载荷下的磨损率[62]
Figure 12. (a) MoS2/Ti3C2Tx composite coating preparation and friction test; (b) Steady state friction coefficient of MoS2/Ti3C2Tx composite coating and steel-to-steel, MoS2 coating on steel and Ti3C2Tx coating on steel; (c) Wear rate of MoS2/Ti3C2Tx composite coating under different loads[62]
图 13 (a) 聚多巴胺(PDA)-3-氨基丙基三乙氧基硅烷(KH550)-Ti3C2Tx填料制备流程；(b) 纯丁腈橡胶(NBR)、Ti3C2Tx/NBR、PDA-Ti3C2Tx/NBR和PDA-KH550-Ti3C2Tx/NBR平均摩擦系数与磨损率[68]
Figure 13. (a) Preparation process of PDA-KH550-Ti3C2Tx filler; (b) Average coefficient of friction and wear rate of pure NBR, Ti3C2Tx/NBR, PDA-Ti3C2Tx/NBR and PDA-KH550-Ti3C2Tx/NBR[68]
PDA—Polydopamine; KH550—3-aminopropyl trie-thoxysilane; NBR—Nitrile butadiene rubber; M—MXene; MP—MXene-PDA; MPK—MXene-PDA-KH550
图 14 (a) 电解质中Ti3C2Tx的浓度分别为0、26、40 mg/mL时制备的Ti3C2Tx/Cu 复合材料摩擦系数随循环次数的变化规律；(b) 各实验组的磨损率及磨损区域SEM图像[73]
Figure 14. (a) Friction coefficient with the number of cycles of Ti3C2Tx/Cu composites prepared when the concentration of Ti3C2Tx in electrolyte is 0, 26, 40 mg/mL, respectively; (b) Wear rate and SEM images of wear area of each experimental group[73]
表 1 Ti3C2Tx作为液体润滑剂添加剂的润滑机制
Table 1. Lubrication mechanism of Ti3C2Tx as liquid lubricant additives
Base lubricant Friction pair Lubrication effects Lubrication mechanism Ref. Paraffin oil Ball 440-C-disk 45# COF: 50% decrease Ti3C2Tx nanosheets enter the friction surface to promote the formation of a continuous uniform lubrication film, micro-polishing and self-healing of the wear area. [38] 100SN base oil Ball 440-C-disk 45# COF: 10%-25%
decreaseTi3C2Tx nanosheets promote the formation of low shear stress lubrication film on the friction surface. [39] PAO8 base oil Ball 32100 steel-
disk 32100 steelCOF: 9% decrease;
Wear volume: 92.3%
decreaseTi3C2Tx nanosheets promote the formation of low shear stress lubrication film on the friction surface. [40] PAO8 base oil Ball 32100 steel-
disk 32100 steelCOF: 31% decrease Enhance the bearing capacity of the lubrication film. [54] Castor oil Ball steel-disk steel COF: 27.9% decrease;
Wear rate: 55.1%
decreaseThe phosphoric acid group of TDPA binds to the hydroxyl group on the surface of Ti3C2Tx, while the long chain alkyl group penetrates into the oil molecules, allowing Ti3C2Tx to be stably dispersed in the oil. Ti3C2Tx promotes the formation of a lubrication film with low shear stress. [42] PFPE Ball GCr15 steel-
disk GCr15 steelCOF: 7% decrease;
Wear rate: 75.3%
decreaseTi3C2Tx nanosheets grafted with fluoropolymer have good dispersion and stability in lubricant. The physical adsorption film of Ti3C2Tx and the tribochemical reaction film together form a continuous and stable lubrication film to separate the contact surface and reduce friction. Ti3C2Tx reduces the decomposition of PFPE at high temperatures. [43] PAO base oil Ball AISI 52100 steel-
disk AISI 52100 steelCOF: 74.6% decrease;
Wear volume: 88.1%
decreaseThe Ti3C2Tx nanosheets loaded with Cu nanoparticles are easier to slide between layers. The physical adsorption film and friction oxide film together form a continuous and stable lubricating film. Cu nanoparticles repair interfacial wear areas. Ti3C2Tx nanosheets were used as growth carriers to avoid agglomeration of Cu nanoparticles. [45] Water Ball AISI 440 C steel-
disk AISI 440 C steelCOF: 20% decrease;
Wear volume: 48%
decreaseTi3C2Tx adsorbs friction surfaces to form a lubrication film with low shear stress, filling in worn areas. [46] Water Ball SiC-
disk 316 steelCOF: 34.74% decrease;
Wear volume: 45.58% decreaseTi3C2Tx adsorbs the friction surface to form a lubrication film with low shear stress, while improving the wettability of water to the steel pan. [47] Water/
glycerolBall Si3N4-
disk sapphireSuperlubrication
(COF: 0.002)
Wear volume: 97.87% decreaseTi3C2Tx forms a physical adsorption film and a friction oxide film composed of titanium and silicon oxide colloids and constitutes a continuous and uniform lubrication film. A large number of hydroxyl groups present in glycerol and water are attached to the Ti3C2Tx nanosheet through hydrogen bond interaction, and a hydrated layer is generated on the nanosheet, which further reduces the shear stress of the liquid film and achieves super-lubrication. As shown in Fig.9. [48] Notes: PFPE—Perfluoropolyether; TDPA—Tetradecylphosphonic acid. 
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表 2 Ti3C2Tx作为固体润滑涂层的润滑机制
Table 2. Lubrication mechanism of Ti3C2Tx as solid lubricating coating
Base lubricant Friction pair Lubrication effects Lubrication mechanism Ref. Ti3C2Tx Ball AISI 52100 steel-
disk Cu
(Ti3C2Tx coating)COF: 75.1% decrease;
Wear volume: 94.9% decreaseTi3C2Tx nanocoatings promote the formation of carbon transfer film to with friction pairs. [57] Ti3C2Tx Ball 100Cr6 steel-
disk 100Cr6 steel
(Ti3C2Tx coating)COF: 35.9% decrease;
Wear volume: 53.8% decreaseDense Ti3C2Tx forms a low shear stress lubrication film, reducing friction and wear. [58] Ti3C2Tx/EP Ball GCr15 steel-
disk Ti-6Al-V
(Ti3C2Tx/EP coating)COF: 34% decrease Ti3C2Tx nanosheets and EP form a stable transfer lubrication film with good adhesion and lubrication properties. [63] Ti3C2Tx/nano-
diamondBall PTFE-silicon chip (Ti3C2Tx/nano-
diamond coating)COF: 50% decrease;
Nearly zero wearThe protective and self-lubricating effect of PTFE, the rolling of nano-diamond, the shear slip of Ti3C2Tx nanosheets and the synergistic effect of various mechanisms achieve low friction and ultra-wear-resistant lubrication. [60] Graphene/
Ti3C2TxBall stainless steel
(DLC coating)-
Silicon chip
(Graphene/Ti3C2Tx
coating)Superlubrication
COF: 0.0042;
Wear rate: 95.5%
decreaseTi3C2Tx nanosheets work collaboratively with graphene to form a lubrication film with low shear stress, while the graphene coating protects the DLC coating of the steel ball. [61] MoS2/Ti3C2Tx Ball AISI 52100 steel-
disk AISI 52100 steel
(MoS2/Ti3C2Tx coating)Superlubrication
COF: 0.0034;
Wear rate: 95.5%
decreaseA strong friction film is formed under high contact pressure. Ti eliminates the harmful effects of oxygen on the lubrication performance of MoS2. [62] Notes: EP—Epoxy resin; PTFE—Polytetrafluoroethylene; DLC—Diamond like carbon.
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表 3 Ti3C2Tx作为复合材料增强相的润滑机制
Table 3. Lubrication mechanism of Ti3C2Tx as composite reinforcement phase
Base lubricant Friction pair Lubrication effects Lubrication mechanism Ref. Ti3C2Tx/UHMWPE Pin steel-disk
Ti3C2Tx/UHMWPECOF: 31.2% decrease Ti3C2Tx spalling during the friction process to form a lubricating film. The addition of Ti3C2Tx improves the hardness and crystallinity of the matrix, and improves the mechanical properties and wear resistance. [67] PDA-KH550-
Ti3C2Tx/NBRBall GCr15 steel-
disk PDA-KH550-
Ti3C2Tx/NBRCOF: 16% decrease;
Wear volume: 76% decreaseThe Ti3C2Tx nanoparticle forms a lubricating film on the wear surface. The surface modification of Ti3C2Tx improves the interface bonding strength and hardness between Ti3C2Tx and matrix, and inhibits abrasive wear and adhesive wear.
[68]Ti3C2/EP Ball GCr15 steel-
disk Ti3C2/EPCOF: 76.3% decrease;
Wear volume: 67.3% decreaseThe addition of Ti3C2Tx nanosheet improves the hardness and thermal conductivity of the material, reduces the deformation and damage during friction, and reduces the defects caused by heat accumulation. [69] Al2O3@Ti3C2Tx/EP Ring GCr15 steel-plate Al2O3@Ti3C2Tx/EP Superlubrication;
Wear volume: 97% decreaseThe sliding interface of Ti3C2Tx, EP and Al2O3 adhere to the metal surface to form a strong lubricating film, which inhibits the oxidation of the steel surface. Al2O3 in friction film induces carbon element to transform into carbon film. [70] Ag@Ti3C2Tx/EP Ball 304 steel-disk Ag@Ti3C2Tx/EP COF: 14.3% decrease;
Wear volume: 87.5% decreaseTi3C2Tx and Ag nanoparticles promote the formation of a continuous and stable friction film, as shown in Fig.15. [78] Ti3C2Tx/Al Ball GCr15 steel-
disk Ti3C2Tx/AlCOF: 59.2% decrease Ti3C2Tx forms a lubricating film on the friction surface and reduces the friction coefficient. Ti3C2Tx improves the hardness of the composite and inhibits abrasive wear. [72] Ti3C2Tx/Cu Ball GCr15 steel-
disk Ti3C2Tx/CuCOF: 46% decrease;
Wear volume: 95% decreaseThe worn surface forms a dense lubricating film rich in Ti3C2Tx. [73] Note: UHMWPE—Ultrahigh molecular weight polyethylene.
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