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Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

Titanium alloys are used as human implant materials in a large number of clinical medical applications such as bone replacement, artificial joints, and dental implants because of their low modulus of elasticity, good biocompatibility, and excellent corrosion resistance [1] [2-3]. The corrosion resistance of untreated titanium alloys depends on the thin and dense oxide film on the surface, however, in practice titanium alloys are susceptible to corrosion by halogen ions [4-6], which will lead to the dissolution of the titanium oxide film and the formation of soluble halides [7]. As implants, titanium alloys are widely used in hip and knee joints, but under the complex mechanical and physiological environment of the human body, the joint surfaces can experience severe corrosion and wear, which can cause inflammation, joint fibrosis, discoloration, and other problems, resulting in shortened implant life [8-9].

(Ti-6Al-2.5Mo-1.5Cr-0.5Fe-0.3Si) TC6 is a kind of two-phase titanium alloys with complex microstructure , with the advantages of low density, high strength, corrosion resistance, but the material cost is expensive, difficult forging processing forming.
Ordinary annealed state TC6 titanium alloy under 300 °C / 5000 h has a good organization and performance stability, different temperature transient high temperature properties such as tensile, creep and lasting and double annealing and isothermal annealing state. By the normal annealing treatment of TC6 titanium alloy semi-finished products can satisfy the use of aircraft structure temperature (below 300 °C).

Grade

Chemical composition (WT %)

TC6

Ti

Fe

C

N

H

O

Mo

Cr

Al

Si

Other

Each

Total

Bal

0.2-0.7

0.1

0.05

0.015

0.18

2.0-3.0

0.8-2.3

5.5-7.0

0.15-0.40

0.1

0.4

Grade

Tensile Requirements

TC6

Tensile strength

(Mpa) min

Yield Strength

(Mpa) min

Elongation

A % min

Reduction of area

Z % min

980

840

10


25


To improve the surface strength and wear resistance of titanium alloys, ion implantation [10], thermal spraying [11], and carburization [12] are often used. Many researchers have also focused on the corrosion wear properties of modified layers of titanium alloys.Sáenz et al [13] prepared Ti-C-N coatings on the surface of Ti6Al4V alloy using PVD technique and found that the nanocrystalline graphite and amorphous carbon structures formed in the coatings had good friction reduction effects and improved the frictional properties of the material in simulated body fluids.Wang [4] studied the corrosion behavior of TiN coatings in fluorinated artificial saliva corrosion behavior and found that the coating has better chemical stability compared with the natural passivated layer and can protect the base titanium ions from migration, but the bond strength of the coating to the substrate is lower.Zhou et al [14] synthesized TiO2 coating on TC4 alloy by microarc oxidation method and the friction factor of the coating was reduced and the wear was decreased compared with the untreated TC4 alloy in the SBF simulated body fluid. Laser shot peening of Ti6Al4V alloy by Mudan [15] was able to promote self-repair of dissolved ruptured oxide film on the alloy surface and showed good corrosion resistance in Hank′s simulated body fluid, but its surface roughness increased after treatment. There is relatively little literature on biocorrosive wear of carburized layers of titanium alloys.

Liu Jing et al [16-17] proposed a double-pulse gas carburizing technique based on induction heating, which is based on the principle of using induction magnetic field to produce skin effect on the metal surface to obtain high-temperature gradient nonequilibrium organization for fast carburizing. In this paper, the organization of the vacuum induction carburized layer of TC6 alloy is characterized, and the corrosion and wear behavior of the carburized alloy in three different environmental media, 0.1% HF, 0.9% NaCl and artificial simulated bodyfluids (SBF), is systematically investigated.

Materials and methods

The test material is TC6 alloy (the mass fraction of its chemical composition is Al:5.5%~7.6%, Mo:2.0%~3.0%, Cr:0.8%~2.3%, Fe:0.2%~0.7%, Si:0.15%~0.40%, C≤0.10%, N≤0.05%, O≤0.15%, H≤0.015% and the balance of Ti), and the sample Before carburizing the specimen, the surface was ground, polished and cleaned. The carburizing process is shown in Fig. 1. The specimen is put into the induction heating reaction furnace for vacuum treatment, heated to the target temperature, and treated with CH4 at -70 kPa as the carburizing medium for 10 min of strong carburizing and 5 min of diffusion in an alternating cycle for 1 h. After that, the sample is cooled to room temperature with the furnace.
The physical phase of the carburized layer on the surface of TC6 alloy was analyzed by using XPertPro X-ray diffractometer (XRD); the cross-sectional hardness distribution was tested by automatic micro hardness tester. In combination with a reciprocating corrosion and wear tester and an electrochemical workstation, Al2O3 balls (Φ = 7 mm,2300 HV) were used as counter-abrasive parts for sliding friction tests in distilled water, 0.1% HF, 0.9% NaCl solution and SBF solution (see Table 1 for composition), and the pure wear amount Vm was expressed using the wear amount obtained from the wear test of the specimens in distilled water [18]. The normal load of the Al2O3 ball during the test was 2 N with a period of 1 s. The polarization curve (LSV) and open circuit potential (OCV) under the friction condition were tested using Bio-logic electrochemical workstation, and the corrosion potential and corrosion current were calculated by Tafel fitting, and the damage mechanism of the surface layer of TC6 alloy under the synergistic effect of corrosion and wear was analyzed; the abrasion marks and roughness of the specimens were characterized by white light interferometry The specimens were characterized by white light interferometer for the morphology and roughness.
20220114035201 99121 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.1 Curve of TC6 alloy carburizing process
Table.1 Chemical composition of simulated body fluids
20220114040157 63722 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

Results and Analysis

Phase structure and microstructure morphology

Figure 2 shows the XRD pattern of TC6 alloy after carburizing. From the figure, it can be seen that TC6 alloy can form a layer of multiphase organization containing TiC on the surface after carburizing. Since the vacuum carburizing process destroys the original natural passivation film of titanium alloy, and the newly formed carburized layer is not a single TiC ceramic phase, the surface area of titanium alloy is prone to secondary oxidation after sampling, so the TiO2 peak appears in the XRD pattern.
20220114040352 10007 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.2 XRD analysis of TC6 alloy
Figure 3 shows the metallographic organization of the TC6 alloy matrix and the vacuum induction carburizing sample at 910°C. During the induction carburizing process, the methane decomposes the active carbon atoms and titanium atoms and the alloying elements react to form a mixed compound phase. Since the radius of carbon atoms (less than 0.077 nm) is smaller than that of titanium (0.147 nm), carbon can easily diffuse on the titanium surface to form compounds with titanium [19-20]. As can be seen from Fig. 3, the original sample in the annealed state is mainly a fine striped α+β complex phase organization; after carburization, a layer of uniform striped white bright organization of about 50 μm is generated on the surface of the specimen and distributed inward perpendicular to the surface (as shown in Fig. 3(b)), which is combined with the XRD pattern: the layer is mainly dominated by the TiC phase. It is followed by a gradient diffusion layer of about 50 μm, and the white-bright tissue gradually decreases. After carburizing at 910°C, the organization from the surface to the heart is TiC-rich layer, diffusion layer and matrix in order. Carbon is one of the α-phase stabilizing elements [21],and due to the high carbon concentration in the most superficial layer, when the active carbon atoms adsorb and penetrate the original surface passivation zone, they form the carbon-rich compound phase by diffusion to the surface layer, which has good corrosion and wear resistance [19]. After the formation of the carbide layer, the carbon concentration of the diffusion layer is much lower than the carbon concentration of the surface layer because the inward diffusion of the active carbon atoms is hindered, and the carbide phase formed is rapidly reduced, and some carbon atoms eventually exist in the matrix by interstitial solid solution, forming a gradient diffusion layer. In addition, the significant temperature gradient caused by the skin effect of electromagnetic induction heating and the diffusion channel provided by the original strip-like α+β phase interface of the alloy accelerate the formation and growth of the carbide layer and diffusion layer, and finally form the gradient complex phase organization of TiC+α′ solid solution phase + matrix α+β.
20220114040544 53452 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.3 Section metallographic structure of TC6 alloy

Cross-sectional hardness analysis

Figure 4 shows the cross-sectional microhardness distribution of TC6 alloy before and after carburization. It can be seen from the figure that after carburizing at 910℃, the surface hardness reaches 850HV0.25, which is nearly 2.3 times higher than that of the original sample, and the penetration depth of carbon atoms is comparable to that of the metallographic analysis in 2.1, and the effective hardening layer (>550HV) is 35μm. Since the phase transition temperature of titanium is 882.5℃, when the carburizing temperature is 910℃, the dense hexagonal structure in TC6 alloy changes to the body-centered The dense density decreases from 0.74 to 0.68, which provides more possibilities for more carbon atoms to enter the interstices and promotes the strengthening of the substrate.
20220114040710 63609 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.4 Section microhardness of TC6 alloy

Corrosion wear behavior

Open circuit potential and friction factor

Fig. 5 shows the open circuit potential and friction factor as a function of time for the sliding wear of TC6 as is and carburized samples in three different media: 0.1% HF, 0.9% NaCl and SBF. As can be seen from the figure, in the three media, the open circuit potential of the original sample and the carburized sample remained stable at rest, and the potential of the carburized sample was higher than that of the original sample; after the start of wear, the open circuit potential of the original sample decreased rapidly, and then the potential increased slowly with time, which was probably due to the destruction of the oxide film on the surface of the titanium alloy during the wear process, which exposed the matrix with activity and accelerated the corrosion of the alloy, making the corrosion potential decrease; subsequently, the sub-surface layer with active matrix also rapidly passivated, and then film, making the potential gradually rise again to a relatively stable value. In the 0.1% HF solution, the original sample can not form a passivation film, so the potential drop is not obvious; while the carburized sample potential drop is larger, mainly because of the strong penetration of F- ions, carburized titanium alloy surface layer is the most dense, the dense density is destroyed by wear, resulting in its potential drop; in comparison, in the acid containing F- ions, the corrosion rate is greater than the passivation rate, so the halogen ions first with the passivation layer (passive protective layer) and thus the potential drops; at 2300s, the open circuit potential drops sharply again, probably due to the destruction of the carburized layer. In the SBF solution, the potential of the original sample dropped rapidly to -1V after the start of wear, mainly due to the destruction of the naturally formed TiO2 layer, which eventually exposed the subsurface active substrate, resulting in a high potential in the micro-abrasion zone (anode) and a low potential in the fully exposed substrate zone (cathode), which formed a certain potential difference between the two and accelerated the corrosion process; the open circuit potential of the carburized sample did not drop much during the wear process. This is because the existence of the surface carburized layer makes the TC6 alloy have high hardness and good corrosion resistance, which can effectively improve the frictional properties of the metal. After the end of wear, the parts subjected to friction are passivated into film rapidly (repassivation process), and the equilibrium mechanism between passivation and corrosion is broken, and the potential of the original sample and carburized sample rises rapidly.
In 0.1% HF solution, the friction factor of the original sample fluctuates around 0.49, which is smaller than that in 0.9% NaCl and SBF solutions; while the friction factor of the carburized sample gradually increases during the corrosion and wear process. In the 0.9% NaCl solution, the friction factor of the original sample fluctuated more during the corrosion and wear process and varied around 0.51, while the friction factor of the carburized sample increased slowly with time. In the SBF solution, the friction factor of the original sample was larger and the average value was around 0.57, while the friction factor of the carburized sample changed smoothly throughout the wear stage and reached a stable friction state with a friction factor of about 0.48. The friction factor of the TC6 alloy decreased after carburization, indicating that the carburization treatment had a good friction reduction effect.
20220114040858 18672 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.5 OCP and COF curves of TC6 alloy in different media
From the friction factor curves, it can be seen that the carburized samples have a low friction factor zone at the beginning of the friction phase, which increases rapidly after a certain period of time, and the low friction factor zone is longer in HF acid, because the corrosion rate is higher than the passivation rate in the acid containing F-ions, and the abrasive particles generated during the wear process are also dissolved, so the pre-wear and wear phases of the specimens are longer. The friction factor of the carburized samples in the three media increased slowly with time, which was due to the increase of the roughness in the grooves and the increase of the friction factor due to the generation of the third body particles during the wear process, while in the HF solution the roughness of the surface of the abrasion marks was reduced due to the occurrence of galvanic corrosion that dissolved the bumps in the grooves (see Table 3 for the roughness), thus the friction factors of the original samples and the carburized samples in the HF acid solution were lower than those of the other two media. Among the three media, the friction factor of the original sample is higher than that of the carburized sample, and the fluctuation range is larger (0.45-0.75), while that of the carburized sample is relatively smooth, which is due to the fact that the α and β phases in the original sample are soft phases with high specific strength but poor wear resistance, and the surface is plowed and dislodged under the action of friction, and the particles formed in the abrasion marks make the friction factor fluctuate [22-23].

Polarization curves

Figure 6 shows the polarization curves of TC6 alloy carburized samples in three different corrosive media with the original samples in static and frictional conditions, and the data obtained by Tafel fitting are shown in Table 2. As can be seen from the figure, the carburized samples have higher corrosion potentials in all three media, indicating that the carburizing treatment can effectively improve the corrosion resistance of TC6 alloy. Compared with the initial static corrosion potential, the corrosion potential during the friction process are reduced, mainly due to the frictional force to destroy the stable state of the surface layer, exposing the fresh surface, the adsorption of ions in solution has a catalytic effect, thus reducing the corrosion resistance. In the carburized samples, the polarization current fluctuates less during the wear process due to the low conductivity of the TiC-rich carburized layer itself.
20220114040955 23803 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.6 potentiodynamic polarization curves of TC6 alloy in different media under dynamic and static conditions
Table 2 polarization curve fitting results
20220114041106 12034 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
In the 0.1% HF solution, the static corrosion polarization curve of the carburized sample was obviously shifted to the left compared with the original sample, and the corrosion potential increased from -1.02V to -0.66V, indicating that the corrosion tendency of TC6 alloy after carburizing at 910℃ was greatly reduced compared with the original sample. As the wear proceeds, the surface layer of the carburized sample is damaged locally due to the interaction between F- and wear, and the surface activity is increased and the equilibrium potential is reduced, thus accelerating the corrosion process; whereas the original sample has been in the activated state in HF solution, and there is no significant change in the polarization curve during the wear process. In the 0.9% NaCl solution, the static corrosion potential of the carburized sample (-0.35 V) was substantially higher than that of the original sample (-0.98 V), and the corrosion current density was also an order of magnitude lower than that of the original sample; after the start of wear, both showed a decrease in potential and an increase in current density. In the SBF solution, the polarization curve of the carburized sample and the original sample showed the same trend, the corrosion potential of the original sample decreased from -0.67V at static corrosion to -1.02V at corrosion and wear, and the corrosion current density increased by an order of magnitude. The reason for this is that the friction causes the corrosion products formed on the surface layer to fall off resulting in the appearance of a new surface, which has a facilitating effect on the adsorption of ions in the solution. The carburized sample has better corrosion resistance than the original sample due to the chemical inertness and higher hardness of the TiC compound on the surface layer [24], which makes it better than the original sample under the synergistic effect of corrosion and wear.

Wear rate and wear mechanism

To analyze the frictional properties of the carburized layer, the wear rate was calculated using the following equation.

20220114041225 80626 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

In the formula: I denotes the wear rate, dv denotes the wear amount, cm3; dt denotes the wear time, h; df denotes the load size, N. Figure 7 shows the histogram of corrosion wear loss of TC6 alloy in different media. As can be seen from the figure, the wear rates of the carburized samples are all smaller than the original samples, indicating that the wear resistance of the titanium alloy can be effectively improved by vacuum induction carburization treatment. From the comparison of wear in distilled water and corrosion solution, it can be seen that the damage of TC6 alloy is intensified under the synergistic effect of corrosion and wear. Among them, the difference of corrosion and wear rate in 0.9% NaCl solution and SBF solution is not much, while the corrosion and wear resistance of TC6 alloy as is and carburized samples in 0.1% HF solution are the worst, and the wear rate is much greater than the other three media. It means that the damage effect of F- on the surface layer of titanium alloy specimen is relatively significant.
20220114041343 30382 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.7 Wear rate of TC6 alloy original sample and carburized sample in different media
Fig. 8 shows the three-dimensional morphology and profile curves of TC6 alloy original sample and carburized sample after wear in the four media. It can be seen from the figure that the surface roughness of the alloy increases after carburization, but due to the increase of hardness, only the raised part is contacted and slightly worn during the wear process, thus the wear amount is smaller and the friction factor is lower than that of the original sample in general. In different media, the TC6 alloy without carburizing treatment formed deeper furrows on the worn surface and grinding was attached in the furrows, while the carburized TC6 alloy had only a few shallow furrows on the worn surface compared to the original sample, which was smooth. This is due to the softness of the TC6 alloy matrix itself, which increases the occlusion between the grinding surfaces and causes a large amount of grinding during the wear process and adheres to the ball and the alloy surface, and the wear mechanism is mainly adhesive wear [25]; while the TiC ceramic phase on the surface of the carburized specimen has a high hardness, which can effectively slow down the cutting effect of the Al2O3 ball on the surface, and the grinding during the wear process will reduce the contact surface area between the abrasive surfaces, and its wear mechanism is mainly abrasive wear [26]. In distilled water, the shallowest abrasion marks of the carburized TC6 alloy were about 1.37 μm; while the original sample reached 19.63 μm, which was 14 times more than the carburized sample (Table 3). In the 0.1% HF solution, corrosion was the main factor causing material loss. From Figure 8(c), it can be seen that the wear marks on the whole surface of the original sample are more uniform, which is due to the formation of corrosion cells in the corrosion solution for the raised and depressed parts in the plow furrow, and the raised area is corroded rapidly under the action of F-. At the same time, the unworn area is relatively shallow and the roughness of the original sample and the carburized sample is the lowest due to the occurrence of faster overall corrosion, thus in 0.1% HF solution. In 0.9% NaCl solution, the original sample produced deeper, wider and uniformly ordered furrows during the friction process, with a relative abrasion depth of 15.72 μm; the abrasion pattern of the carburized sample in 0.9% NaCl solution is shown in Fig. 8(f), with a less damaged surface and a relative abrasion depth of 8.11 μm. Combined with the corresponding open-circuit potential, the incompleteness of the carburized layer resulted in a lower potential, but the corrosion resistance was less than that of the original sample. However, the corrosion resistance is still better compared to the as-received sample. In the SBF solution, the relative abrasion depth is 15.04 μm due to the influence of Cl-, HPO2-4, and H2PO-4 plasma in the SBF solution, and plastic deformation occurs at the localized location of the abrasion marks. As shown in Fig. 8(h), the surface of the carburized TC6 alloy was less abraded than the original sample, and the relative abrasion depth was 7.76 μm, indicating that the presence of the carburized layer could better inhibit the damage to the internal matrix by various ions in the SBF solution.
20220114041442 19715 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Fig.8 three dimensional morphology and contour curve of TC6 alloy after wear
Table 3 wear mark parameters of TC6 alloy in different media
20220114041528 64478 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

Corrosion-wear synergy

When a material undergoes wear action in a corrosive environment, chemical, electrochemical and mechanical factors act together on the material surface [27] , and thus the total wear amount Vt of the material should be equal to the sum of the pure corrosion amount Vc, the pure wear amount Vm and the corrosion-wear interaction amount ΔV [28] . That is.

20220114041827 58494 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

In turn, the corrosion-wear interaction volume ΔV consists of the wear-promoted volume ΔVc and the corrosion-promoted volume ΔVm. Namely.
Therefore.
20220114041841 90478 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Where.
20220114041906 34075 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Formula: Vcorr is the amount of volume loss caused by corrosion, can be calculated by Faraday formula, the formula is as follows
20220114041929 79132 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media
Formula: t is the time of corrosion wear, F is the Faraday constant (96,500C-mol-1), ρ is the density of TC6 alloy, M is the relative atomic weight of titanium alloy, n is the chemical valence of titanium elements. Table 4 lists the wear fractions of the TC6 alloy before and after carburization.
By calculating each component of the corrosion and wear process, it can be seen that the proportion of material loss (ΔV/Vt) caused by corrosion and wear interaction in 0.1% HF solution, 0.9% NaCl solution and SBF solution for the original sample are 90.9%, 38.4% and 33.3%, respectively, and for the carburized sample: 85.9%, 59.7% and 46.1%. In the 0.1% HF solution, the ΔV/Vt was the highest for both the original sample and the carburized sample, indicating that corrosion has a significant role in promoting wear in 0.1% HF acid, and the corrosion-wear interaction is the main factor causing material loss of TC6 alloy. In 0.9% NaCl solution and SBF solution, the ΔV/Vt of the original sample is significantly lower, indicating that the material loss in these two media is mainly caused by mechanical wear; for the carburized sample, its ΔV/Vt is also slightly lower, but the percentage is still larger. Comparing the Vm values of pure wear of the titanium alloy in distilled water, the pure wear of the titanium alloy carburized at 910°C was reduced by 37% compared to the original sample. In the material loss caused by corrosion wear interaction, the amount of corrosion promotion by specimen wear (ΔVc) is lower.
Table 4 corrosion wear components and proportions of TC6 alloy
20220114041737 42185 - Corrosion and wear properties of carburized layer of TC6 titanium alloy in different media

Conclusion

  • (1) After vacuum induction carburization of TC6 alloy, the cross-sectional organization from the outside to the inside of the alloy consists of carbide-rich layer (TiC), diffusion layer and matrix, and the hardness of carbide-rich layer reaches 850 HV0.25, which is 2.3 times higher than that of the matrix. The penetration depth of carbon atoms reached 62.5μm, and the effective penetration layer was 35μm.
  • (2) In the three media, the original TC6 alloy surface oxide film broke under the action of friction, and the corrosion tendency increased, and the corrosion potential of the carburized alloy increased and the corrosion current density was significantly lower than that of the original sample. In the corrosion and wear process, the wear mechanism of the original sample is adhesive wear, while the wear mechanism of the carburized sample is abrasive wear, and the carburized titanium alloy shows a smaller friction factor and wear rate.
  • (3) For the material loss in the corrosion wear process, the pure wear of the carburized alloy in distilled water was reduced by 37% compared with the original sample. The carburized sample in 0.1% HF solution had the highest percentage of corrosion wear interaction with the original sample. The promotion of wear by corrosion is the main factor causing material loss.

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