3.4. SEM Analysis of Worn Surfaces
Figure 6 shows the SEM images of wear spots corresponding to blank lubricating grease and lubricating grease with the optimal mass fraction of MoS
2 added in different ways. From
Figure 6a, it can be seen that the wear surface corresponding to the blank grease exhibits obvious friction marks, with wide and large furrows on the wear marks. The wear marks on the steel ball surface (Figures 6b-e) corresponding to the lubricating grease containing the MoS
2 additive become relatively less obvious, and the surface becomes smoother. This may be because MoS
2 has a layered structure that is easy to slide, so it can form a stable film on the rubbing surface under friction conditions, thereby achieving an anti-wear effect.
By comparing Figures 6(b-e), it can be found that the MoS2 grease prepared by the “Method D” shows the shallowest wear marks and the smoothest grinding surface, indicating that the grease prepared by this addition method has the best anti-wear effect. This may be because the addition of MoS2 before thickening allows MoS2 and the base oil to be in contact and mixed for a longer period, and may also have a longer chemical reaction. Moreover, this method adopted a three-roller grinder for grinding, which allows MoS2 to be more evenly distributed in the lubricating grease. Therefore, the MoS2 lubricating grease prepared by the “Method D” exhibits the smallest wear spot diameter and the least obvious friction marks.
3.5. XPS Analysis of Worn Surfaces
In order to reveal the lubrication mechanism of MoS
2 as an additive in lithium grease, the chemical state of elements on the surface of the abrasive spot was analyzed by XPS.
Figure 7 shows the XPS spectra of C1s, O1s, Fe2p, S2p, and Mo3d on the wear surface of steel balls caused by lithium-based grease with 0.01% MoS
2.
The peaks with binding energies of 284.8, 284.98 and 287.18 eV in the C1s spectra (
Figure 7b) correspond to C-C, C-O-C [
15] and C=O [
16] bonds, respectively. The binding energies of O1s (
Figure 7c) at 529.37 and 531.81 eV peaks correspond to metal oxides (Fe
2O
3) and C-O bonds, respectively [
17]. The binding energies of Fe2P (
Figure 7d) at 706.30 and 711.76 eV peaks correspond to FeS
2 and Fe
2O
3, respectively[
18]. The 709.64 and 723.19 eV correspond to Fe 2P
3/2 and Fe 2P
1/2 of FeO, respectively. The peaks of the S2p-XPS spectra (
Figure 7e) at 161.50 and 168.60 eV correspond to MoS
2[
19]/FeS
2 and Metal sulfate, respectively. The peaks at 232.68 and 235.83 eV in the Mo3d-XPS spectra (
Figure 7f) correspond to MoO
2 and MoO
3, respectively[
20]. The appearance of MoO
2 and MoO
3 indicates that the MoS
2 additive has been oxidized during the friction process, that is, MoS
2 may partially undergo tribochemical reactions during the friction process.
3.6. Results of Corrosion Test
To explore the corrosion performance of MoS
2-lithium grease on metal under natural conditions, the corrosion test was conducted with the GCr15-bearing steel sheet.
Table 2 shows the quality changes of the steel sheets before and after 15 days.
The corrosion rate of MoS
2 grease on bearing steel can be calculated according to the following formula [
21]:
Where Δm represents weight loss, A is the surface area of the bearing steel, t is the time of the steel plate buried in the grease, CR represents the corrosion rate, CR0 and CR1 represent the corrosion rate with and without additives, respectively.
Figure 8 shows the corrosion rate of GCr15-bearing steel sheets buried in MoS
2 lubricating grease with different mass fractions prepared by different addition methods for 15 days. Compared with the blank group without MoS
2, it can be found that the addition of MoS
2 additive reduces the corrosion rate of bearing steel in the natural environment, indicating that the addition of MoS
2 effectively slows down the corrosion process of bearing steel.
However, as the addition of additives changes, the content of MoS
2 with the best corrosion inhibition efficiency also changes. The optimal corrosion inhibition efficiency of MoS
2 by the “Method A” was found at 0.01wt% MoS
2 content. When MoS
2 was added by the “Method B”, the optimal corrosion inhibition efficiency occurred when the MoS
2 content was 0.01wt%. When MoS
2 was added by the “Method C”, the optimal additive content for corrosion inhibition efficiency was 0.07wt%. When the “Method D” was adopted to add MoS
2, 0.03wt% MoS
2 exhibited the best corrosion inhibition efficiency. This change may be due to the varying degree of uniform distribution of MoS
2 in the lubricating grease when added in different ways, resulting in different corrosion results. The data in
Table 2 and
Figure 8 both show that when the “Method B” was used to add 0.01wt% MoS
2, the configured grease had the lowest corrosion rate on the bearing steel, that is, the corresponding corrosion inhibition efficiency was the highest, reaching 96.97%.
The SEM image of the GCr15-bearing steel sheet embedded in 0.01% MoS
2 lubricating grease for 15 days is shown in
Figure 9.
Figure 9a shows that no obvious surface coverings or corrosion pits were found on the surface of the original bearing steel sheet. However, the surface of the bearing steel corresponding to the blank grease without MoS
2 showed obvious corrosion, with an unsmooth surface and severe corrosion pits (
Figure 9b).
Figure 9c is the SEM diagram of the surface of the steel sheet caused by 0.01wt% MoS
2 grease prepared by the “Method A”. It can be seen that corrosion pits appear in a small part of the surface of the steel sheet under such circumstances. When 0.01wt% MoS
2 was added using the “Method B”, the resulting grease causes the slightest corrosion on the surface of the steel sheet (
Figure 9d). When 0.01wt% MoS
2 grease was prepared by “Method C”, the corrosion test results in uneven corrosion on the surface of the steel sheet, as shown in
Figure 9e. As can be seen from
Figure 9f, the grease prepared by adding MoS
2 additive with the method of “Method D” will cause local corrosion on the surface of the steel sheet. From Figures 9 (c-f), it can be found that MoS
2 grease has a certain corrosion effect on the steel surface, which may be because the S element in MoS
2 can combine with the Fe element in the bearing steel to produce iron sulfide and other products [
9], so MoS
2 has a certain corrosion effect, and the surface of the steel sheet was therefore pitted. However, by comparing
Figure 9b and Figures 9 (c-f), it can be found that after the addition of MoS
2 additive, the corrosion phenomenon on the surface of the bearing steel was slowed down in different forms, indicating that MoS
2 has a certain corrosion inhibition effect.
To better demonstrate the morphology and roughness of GCr15-bearing steel sheets after corrosion experiments, three-dimensional (3D) morphology studies were also conducted on the corroded steel sheets.
Figure 10 shows the 3D morphology of the steel sheet after being embedded in 0.01% MoS
2 grease for 15 days.
From
Figure 10a, it can be observed that the surface roughness of the original bearing steel was 0.034 μm. After 15 days of embedding with blank lubricating grease without MoS
2, the surface roughness of the bearing steel was the highest, reaching 0.223 μm (
Figure 10b).
Figure 10c illustrates that the surface roughness of the corroded steel plate corresponding to the lubricating grease prepared by the “Method A” was 0.113 μm.
Figure 10d shows that the roughness of the corroded steel surface corresponding to the lubricating grease prepared by the “Method B” was 0.047 μm.
Figure 10e and 10f represent the 3D images of the corroded steel surface corresponding to the lubricating grease prepared by the “Method C” and the “Method D”, respectively, with a surface roughness of 0.193 μm and 0.054 μm.
Comparing
Figure 10b and Figures 10 (c-f), it can be found that regardless of the method of adding 0.01wt% MoS
2, the formulated lubricating grease will reduce the surface roughness of bearing steel after corrosion. The adoption of the “Method B” resulted in the maximum reduction of surface roughness (
Figure 10d) by 0.176 μm. The method of “Method C” (
Figure 10e) with the least reduction in surface roughness resulted in a reduction of only 0.03 μm. The 3D morphology in
Figure 10 is in good agreement with the SEM results in
Figure 9. This further indicates that adding MoS
2 additive can slow down the corrosion rate of bearing steel and can protect the corrosion of the device for a long time under natural conditions.