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Microstructure and wear behavior of TiAl3 matrix self-lubricating composites by addition of fluoride solid lubricants

  • Shouren Wang EMAIL logo , Yingzi Wang , Liying Yang , Linghui Song and Peilong Song
Published/Copyright: September 7, 2013
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Science and Engineering of Composite Materials
From the journal Science and Engineering of Composite Materials Volume 21 Issue 3

Abstract

The microstructure of TiAl3 composites with addition of different weight contents of solid lubricant (LiF, NaF, CaF2, and 38% CaF2-62% BaF2) were observed by scanning electron microscopy. Hardness, bend strength, and fracture toughness tests were carried out on an electron omnipotence testing machine. The friction and wear tests were performed using a high-temperature pin-on-disc tribometer at different friction conditions such as different loads, different sliding speeds, and different working temperatures. The results show that TiAl3 composites with 38% CaF2-62% BaF2 solid lubricant exhibit higher bending strength and fracture toughness than composites with other solid lubricants. In addition, the wear rate of TiAl3 composites with 38% CaF2-62% BaF2 solid lubricant is lowest in all composites. It is attributed to 38% CaF2-62% BaF2 solid lubricant forming a compact film on the wear surface of TiAl3 composites. The compact-film-forming mechanism is attributed to fluoride particles forced out of the reservoirs due to its high thermal expansion coefficient.

Keywords: mechanical properties; microstructure; solid lubricants; TiAl3; wear rate

1 Introduction

TiAl3 intermetallic alloys have intrinsic characteristics such as low density (3.3 g/cm3), high elastic modulus (216 GPa), high creep strength (up to 900°C), high melting point (1350°C), and excellent chemical stability, which make them promising candidates for wear-resistance components [1–4]. They have excellent prospects for tribological applications especially under elevated temperature conditions. Many components such as gas turbine blades, engine exhaust valves, tappets, valve spring retainers, mechanical components in nuclear reactions, etc., demand combinations of high-temperature wear, oxidation, and self-lubrication properties [5]. Thus, there is an ongoing need for developing high-temperature self-lubricating materials with excellent tribological properties accompanied by high mechanical strength [6, 7]. Addition of solid lubricants to matrix is an effective method to decrease the wear rate and wear coefficient. Conventional liquid lubricants and most conventional solid lubricants (e.g., graphite), however, are not suitable for high-temperature environment in which the temperature is above 350°C. Numerous solid materials, such as noble metals (e.g., Au, Ag, Pt), inorganic fluorides (e.g., LiF, CaF2, BaF2), some metal oxides (e.g., NiO, MoO3, the Magneli phases, such as TiO2-γ, etc.), have been employed as solid lubricants [8]. They exhibit a high friction coefficient under the condition of low sliding velocities and poor adhesion to the substrate at temperatures below 260°C; however, some excellent performance was shown at temperatures above 350°C. The mechanism behind their effective lubricating performance is understood to be due to easy shearing along the basal plane of the hexagonal crystalline structures [9]. Owing to the physical (prevents adhesion), chemical (enables tribochemical reactions), and microstructural (lamellar structure with low shear strength) influence of the solid lubricants on a tribological contact of working surfaces, they are effective in reducing friction and wear [10]. There are numerous examples from the literature [11–13] in which CaF2 was used as a solid lubricant to study the mechanical properties and microstructural characterization of composites such as Al2O3/TiC/CaF2, Al2O3/CaF2, and Al2O3/TiC/CaF2 materials. For example, the self-lubricating TiAl-based composite with Al4C3/TiC/CaF2 synthesized by Ni-P electroless plating powder method can provide good friction-reducing and antiwear abilities [5]. Self-lubricating composites doped with solid lubricants of CaF2/BaF2 eutectic and silver in a metal-bonded chromium carbide (Cr3C2) matrix have been developed by plasma spraying and powder metallurgy methods [14, 15]. Tribological properties of laser cladding Ni-Cr-C-CaF2 mixed powders to form a multifunctional composite coating on γ-TiAl substrate were investigated [16]. Yang et al. [17] studied the effect of nanosized Cr2O3 addition on the characteristics of NiCr-Cr2O3-Ag-BaF2/CaF2 coating. However, numerous studies [18–20] focus on the research of film that will form a stable and adherent film. Organic combination of solid lubricants with TiAl3 alloys to develop self-lubricating composites is the development trend of tribological materials. Several researches have been conducted on the friction and wear behaviors of TiAl3-based self-lubricating materials, and most of them have revealed the wear mechanism of such materials. The wear behavior of composites is complicated; however, it is necessary to address the characterization of the TiAl3-based self-lubricating materials and their role on the wear behavior. In the present study, the microstructure and wear resistance of TiAl3 composites with additions of different solid lubricants are discussed. Sliding wear tests against Al2O3 disc were performed on the composites. A relative model of μ-W has been proposed. Detailed observations have been conducted to clarify the formation mechanism of solid lubricant film on matrix. In addition, the effects of solid lubricants on the friction and wear behavior of these composites are also discussed.

2 Experimental

2.1 Materials fabrication processing

The starting powders with composition Ti25Al75 were mechanically mixed in a planetary ball miller (QM-1SP2) using a 500-ml stainless steel jar and 40 g of powders. Fluoride solid lubricants LiF, NaF, and CaF2 and 38% CaF2-62% BaF2 (CB) eutectic solid lubricants were added into the Ti25Al75 matrix. The properties of fluoride solid lubricant are shown in Table 1. The addition amounts of each type of lubricant are 5, 10, 15, and 20 wt%, respectively. Ball milling was carried out in argon atmosphere at 320 rpm for 4 h using Al2O3 balls (10, 5, and 3 mm in diameter). The ball-powder weight ratio is 5:1. The milled powders were densified by hot pressing. Powders were directly cold compacted under a pressure of 250 MPa at room temperature. Degassing occurred up to 200°C under vacuum (vacuum degree, 1×10-1). Samples 30 mm in diameter and about 6 mm in height were prepared.

Table 1

Properties of fluoride solid lubricants.

PropertiesLubricants
LiFNaFBaF2CaF2CB
Molecular weight25.9441.97175.3678.08–
Hardness (Mohs)44444
Density (g/cm3)2.642.784.893.18
Friction coefficient0.07–0.200.07–0.200.07–0.200.07–0.200.07–0.20
Melting temperature (°C)1280842137014701022
Oxidation temperature (°C)700700700–700
Usage temperature (°C)2525250250430–820
Crystal structurebccbccBccBcc–

2.2 Wear and friction tests

The friction and wear tests were performed using a high-temperature pin-on-disc tribometer (XP-5, China) (Figure 1) capable of going up to 350°C and 450°C. All tests were carried out at a linear velocity of 105 mm/s and a load of 50–150 N. The test sample was in the form of cuboids chips (12 mm×5 mm×5 mm) against a rotating disc, which has a dimension of Φ300×10 mm. The samples were cut from the ingot and wet ground with SiC paper down to 1200 grit, which gave an average surface roughness of Ra 0.03 μm. The disc materials were commercially available discs of bearing steel and corundum that were polished to average surface roughness of Ra 0.02 μm. The tangential friction force and friction coefficients were monitored with the help of electronic sensors. The measurement error is ±0.05. These tests were conducted at sliding distance of 388.8 m (sliding time, 60 min). Detailed friction and wear test conditions are listed in Table 2.

Figure 1 Schematic experimental setup for carrying out the wear tests.
Figure 1

Schematic experimental setup for carrying out the wear tests.

Table 2

Friction and wear test conditions.

Work specimenTiAl3, TiAl3+X wt% Y (X=5, 10, 15, 20, 25; Y=LiF, NaF, CaF2, and CB, respectively)
Friction systemPin-on-disc
Test temperature25°C, 350°C, 450°C
Specimen size12 mm×5 mm×5 mm
Disc materialsBearing steel and corundum ceramic disc
Dimension of discΦ300×10 mm
Speed of the disc105 mm/s
Normal load50–150 N
Sliding distance388.8 m

2.3 Characterization and mechanical properties test

Optical microstructures were observed after mechanical polishing with polycrystalline diamond suspension glycol-based solution. The grain structure was revealed by subsequent etching in 7 s with an HF/HNO3/H2O solution in a volume ratio of 1:6:7. The morphology and microstructure of the surface were observed by scanning electron microscopy (SEM) (Model No.S-2500, HITACHI). Chemical element distributions were examined by energy spectrum analyses (EDS, OXFOED INCA). X-ray diffraction (XRD) analysis using Cu Ka radiation was done with D/MAX-2000 equipment (RIGAKU). The density of the sintered samples was measured according to Archimedes’ principle. The room-temperature Rockwell hardness (HRC) of the powders was measured with a 10-N load and 15-s indentation time, averaging at least five tests. The fracture toughness tests were carried out on an electron omnipotence testing machine (Instron5569). The specimens were loaded at a constant crosshead speed of 10-2 cm/s. The notch was cut through electrodischarge machining, which has a geometry characteristic of root radius of 200 μm, normal width of 2 mm, and a normal length of approximately 3–4 mm.

3 Results and discussion

3.1 Microstructures and characterization

Figures 2–5 show the SEM micrographs of self-lubricating composites with different solid fluoride lubricants (LiF, NaF, CaF2, and CB, respectively) and different addition amounts (5%, 10%, 15%, and 20%, respectively). The effects of different solid lubricant amounts on the microstructure of composites are clear – that porosity and relative density change with different addition amounts of fluoride lubricants. It can be shown that porosity increases with increasing amounts of solid fluoride lubricant added. The relative densities of the composites with additions of CB lubricant have a higher densification than others. From Figure 5, it is shown that the surface of TiAl3 composites with lower amounts of solid lubricant exhibits a compact surface. However, it is obvious that there are many pores or cavities located on the SEM surface. With the increase in the amount of CB, the amounts of pores or cavities do not increase distinctly unless it exceeds 20%. CaF2 and BaF2 particles are mostly uniformly distributed throughout the microstructure of composites, and conglomeration occurred in only a small region of the SEM micrographs, shown as black circles in the micrographs.

Figure 2 Microstructure of self-lubricating composites with different LiF addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.
Figure 2

Microstructure of self-lubricating composites with different LiF addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.

Figure 3 Microstructure of self-lubricating materials with different NaF addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.
Figure 3

Microstructure of self-lubricating materials with different NaF addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.

Figure 4 Microstructure of self-lubricating materials with different CaF2 addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.
Figure 4

Microstructure of self-lubricating materials with different CaF2 addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.

Figure 5 Microstructure of self-lubricating materials with different CB addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.
Figure 5

Microstructure of self-lubricating materials with different CB addition amounts: (A) 5%, (B) 10%, (C) 15%, and (D) 20%.

XRD analysis results (Figure 6) indicated that the main matrix phases are TiAl and TiAl3. It can be seen that the fluoride solid lubricants LiF, NaF, CaF2, and CB all existed in the sintered specimens. Moreover, the peaks of fluoride solid lubricant became broader and the intensity became higher with increasing addition amounts of fluoride solid lubricant.

Figure 6 XRD analysis of composites with different fluoride solid lubricants: (A) LiF, (B) NaF, (C) CaF2, and (D) CB.
Figure 6

XRD analysis of composites with different fluoride solid lubricants: (A) LiF, (B) NaF, (C) CaF2, and (D) CB.

3.2 Mechanical properties

The microhardness of TiAl3 composites with different amounts of solid lubricants are shown in Figure 7A. It can be seen that additions of fluoride solid lubricant to TiAl3 matrix led to a decrease in hardness compared to matrix. The decreasing trends of additions of CB are larger than others. The hardness of TiAl3 composites without CB lubricant is 76 HRC, whereas with 20 wt% CB solid lubricant the hardness is 51 HRC. The hardness of CB solid lubricant is lower than that of matrix; thus, the composite without CB solid lubricant has higher hardness than that with much CB solid lubricant.

Figure 7 The effect of addition amounts of different solid lubricants on hardness and bend strength: (A) hardness and (B) bend strength.
Figure 7

The effect of addition amounts of different solid lubricants on hardness and bend strength: (A) hardness and (B) bend strength.

Figure 7B shows the effect of addition amounts of different lubricants on the bend strength of composites sintered at 1200°C. It was found that the bending strength decreased with addition amounts of fluoride solid lubricants except addition of 5%. For CB solid lubricant, the bending strength of composites without solid lubricant is 600 MPa, whereas with 5 wt% solid lubricant the bending strength is 620 MPa and with 20 wt% solid lubricant it is 580 MPa. For LiF solid lubricant, the bending strength with 5 wt% is 602 MPa, whereas with 20 wt% it is 575 MPa. It must be that with the increased addition of fluoride solid lubricants in the matrix, the metallic bond force of the matrix was cut, thus the bend strength decreased.

3.3 Wear behavior

Figure 8 shows the friction coefficient of TiAl3 matrix and its composites with different solid lubricants under the condition of sliding against Al2O3 disc at 450°C. It can be seen that the TiAl3 matrix alloy exhibits higher friction coefficient. For LiF and CaF2 solid lubricants, with the increase in weight fraction of solid lubricants the friction coefficient decreases gradually. However, the decrease in the degree of friction coefficient is different. For example, the friction coefficient value of LiF is from 5% LiF-0.63 to 20% LiF-0.36, whereas that of CaF2 is from to 5% CaF2-0.54 to 20% CaF2-0.40. Moreover, with the increase in sliding time, the friction coefficient of 20% LiF composites has no distinct change, whereas that of 20% CaF2 composites decreases distinctly. For NaF solid lubricants, with the increase in the weight fraction of solid lubricants the friction coefficients show the opposite trend. That is, the friction coefficient of 5% NaF composites is 0.39, whereas that of 20%NaF composites is 0.49. The reason is not clear and this will be discussed in the future. For CB solid lubricants, with the increase in weight fraction of solid lubricants, the friction coefficient decreases gradually. Once the weight fraction of CB solid lubricants exceeds 15%, a distinct increasing trend occurs.

Figure 8 Friction coefficient with different addition amounts of fluoride solid lubricants: (A) LiF, (B) NaF, (C) CaF2, and (D) CB.
Figure 8

Friction coefficient with different addition amounts of fluoride solid lubricants: (A) LiF, (B) NaF, (C) CaF2, and (D) CB.

Figure 9 shows the effect of different weight fractions of different solid lubricants on the wear rates of the TiAl3 composite. It is shown that with the increase in weight fraction of solid lubricants, the wear rate decreases gradually for all solid lubricants. The wear rate of LiF and NaF composite is higher than that of CaF2 and CB composites. The wear rate of CB composites is lowest in all composites. For example, the wear rate value of 10% NaF composites is 1.65×10-4 mm3 N-1 m-1, whereas that of 10% CB composites is 1.1×10-4 mm3 N-1 m-1. With the increase in weight fraction of CB solid lubricants, the wear rate reaches the minimum value of 1.0×10-4 mm3 N-1 m-1 as a function of 15% CB solid lubricants.

Figure 9 Wear rate with different fluoride solid lubricant and different addition amounts.
Figure 9

Wear rate with different fluoride solid lubricant and different addition amounts.

Figure 10 shows the micrograph of the worn surface of the TiAl3 composites with different weight fractions of CB solid lubricants. The worn surfaces of TiAl3 composites with and without CB solid lubricants exhibit a similar morphology showing the existence of rough regions and a few fine scratches. Furthermore, on the worn surface, there are many cracked particles and pullout pits, which resulted from brittle fracture. Moreover, there is more wear debris on the surface of the composite without CB solid lubricant, as the brittle fracture was directly relative to the strength of grain boundaries. It is noticeable that a compact film was formed on the wear surface of TiAl3 composites with CB solid lubricant because fluoride particles were forced out of the reservoirs due to its high thermal expansion coefficient. With increasing weight fraction of CB solid lubricant the glaze film becomes more and more integrated, and less wear debris was observed (Figure 10A–C). It is well known that CB solid lubricant has excellent self-lubricating properties at temperatures higher than approximately 400°C when it undergoes the brittle to ductile transformation, forming a fully ductile phase with very low shear strength. Therefore, addition of CB solid lubricant to TiAl3 matrix can greatly enhance the wear resistance and reduce the friction coefficient of TiAl3 composites.

Figure 10 Worn surfaces of TiAl3-CB materials with different CB content: (A) 0%, (B) 5%, (C) 10%, and (D) 15%.
Figure 10

Worn surfaces of TiAl3-CB materials with different CB content: (A) 0%, (B) 5%, (C) 10%, and (D) 15%.

4 Conclusions

Addition of fluoride solid lubricant to TiAl3 matrix led to a decrease in hardness compared to the matrix. The decreasing trends of addition of CB are larger than others. The bending strength and fracture toughness decrease with increasing amounts of fluoride solid lubricants except addition of 5% lubricant.

TiAl3 matrix alloy exhibits higher friction coefficient and wear rate. With different solid lubricants, the friction coefficients of composites are distinctly different. In addition, with the increase in weight fraction of solid lubricants, the wear rate decreases gradually for all solid lubricants. In all composites, the wear rate and friction coefficient of TiAl3 composites with CB solid lubricant is lowest. It is attributed to CB solid lubricant forming a compact film on the wear surface of TiAl3 composites. The compact-film-forming mechanism is due to fluoride particles forced out of the reservoirs owing to its high thermal expansion coefficient.

Corresponding author: Shouren Wang, School of Mechanical Engineering, University of Jinan, Jinan 250022, P.R. China, e-mail: ;

Acknowledgments

The authors gratefully acknowledge the financial support from the National Natural Science Foundation of China (Grant No. U1134101 and No. 51372101) and Natural Science Foundation of Shandong Province (Grant No. ZR2011EMM003).

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Received: 2013-4-18
Accepted: 2013-8-10
Published Online: 2013-9-7
Published in Print: 2014-6-1

©2014 by Walter de Gruyter Berlin Boston

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

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https://doi.org/10.1515/secm-2013-0102
Keywords for this article
mechanical properties; microstructure; solid lubricants; TiAl3; wear rate
Creative Commons
BY-NC-ND 3.0

Articles in the same Issue

  1. Frontmatter
  2. Original articles
  3. Microstructures and physical properties of laser amorphous reinforced composite coatings
  4. The thermal resistance, flame retardance, and smoke control mechanism of nano MH/GF/NBR composite material
  5. The effect of sodium hydroxide treatment and fiber length on the tensile property of coir fiber-reinforced epoxy composites
  6. Evaluation of morphological characteristics and mechanical performance of Rockforce mineral fiber- and glass fiber-reinforced polyamide-6 composites
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  8. A study on tribological characterization of Al-Cu-Mg-B composites subjected to mechanical wear
  9. Microstructure and wear behavior of TiAl3 matrix self-lubricating composites by addition of fluoride solid lubricants
  10. Mechanical properties of Ni-nano-Al2O3 composite coatings on AISI 304 stainless steel by pulsed electrodeposition
  11. Improvement of Khorasan mortar with fly ash for restoration of historical buildings
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  22. Electrical discharge machining of Al-TiB2 with a low-frequency vibrating tool
  23. Vibration behavior of a radially functionally graded annular disc with variable geometry
  24. Buckling behaviors of the impacted composite plates
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