A fluorinated molybdenum disulfide material and a method of making the same

Abstract

A fluorinated molybdenum disulfide material and a preparation method thereof, the preparation method comprising the following steps: 1) drying molybdenum disulfide at a temperature of 60-150 DEG C, and then placing it in a reactor; 2) preparing fluorination mixed gas with a volume fraction of fluorine gas of 0.1-20%; 3) introducing the fluorination mixed gas prepared in step 2) into the reactor in step 1) at a speed of 0.2-5 L / min until the pressure is 2-80 Kpa, and carrying out fluorination reaction for 10-60 min, and when the reaction is completed, the residual gas in the reactor is removed; 4) repeating step 3) 1-5 times. The preparation method of the fluorinated molybdenum disulfide material has the characteristics of direct fluorination modification and high efficiency and controllability, and replaces unstable hanging bonds (such as oxygen groups) in MoS2 layers, and further forms stable fluorine-containing chemical bonds, so that the oxidation resistance of MoS2 is greatly improved, and the self-lubricating ability is also improved.

Description

Technical Field

[0001] This invention relates to the field of nanomaterials technology, specifically to a molybdenum disulfide fluoride material and its preparation method, which is mainly used in micro-nano devices, nanocomposites, lubrication and other fields. Background Technology

[0002] Molybdenum disulfide (MoS2), a two-dimensional transition metal compound, exhibits unique physical and chemical properties and has been widely used in micro- and nano-optoelectronic devices, nanocomposites, energy storage, catalysis, and lubrication. However, MoS2's poor oxidation resistance leads to its poor stability in complex application environments; once oxidation occurs, its performance deteriorates significantly. Previous studies have shown that the oxidation process of MoS2 involves oxygen attacking Mo and S atoms at edges or defects, forming unstable dangling bonds. These dangling bonds are easily removed during use, exposing more Mo and S atoms, accelerating further oxidation reactions, and ultimately leading to rapid destruction of the MoS2 sheets. Existing research has mainly focused on improving the oxidation resistance of defect-free, high-quality MoS2, but this significantly increases cost and process complexity, thus limiting the large-scale practical application of MoS2.

[0003] Fluorine, the most electronegative element in the periodic table, forms highly stable chemical bonds, making it difficult to further oxidize. In fact, the ability of introducing fluorine to improve the oxidation resistance of materials has been clearly demonstrated in other fields. Particularly in the field of perovskite solar cells, many researchers have introduced fluorine into the perovskite system, significantly improving the oxidation resistance and moisture resistance of perovskite devices, thus ensuring the long-term stable operation of perovskite solar cells (J. Am. Chem. Soc. 2021, 143, 8, 3231–3237; Adv. Energy Mater. 2021, 2101454). Therefore, through controlled fluorination reactions, utilizing fluorine to directionally replace unstable dangling bonds such as oxygen groups in MoS2, thereby forming more stable fluorine-containing chemical bonds, it is expected to improve the oxidation resistance of MoS2 in a low-cost and efficient manner. Summary of the Invention

[0004] This invention addresses the shortcomings of existing technologies by providing a fluorinated molybdenum disulfide material and its preparation method. Utilizing the direct fluorination modification and its highly efficient and controllable characteristics, this invention directionally replaces unstable dangling bonds (such as oxygen groups) within MoS2 sheets, further forming stable fluorinated chemical bonds. This significantly enhances the oxidation resistance of MoS2 and synergistically improves its self-lubricating ability.

[0005] To achieve the above objectives, the present invention provides a method for preparing molybdenum disulfide fluoride material, comprising the following steps:

[0006] 1) Dry molybdenum disulfide thoroughly at 60-150℃, and then place it in the reactor;

[0007] 2) Prepare a fluorinated mixed gas with a fluorine gas fraction of 0.1-20%;

[0008] 3) Introduce the fluorinated mixed gas prepared in step 2) into the reactor in step 1) at a rate of 0.2-5 L / min until the pressure is 2-80 kPa, and carry out the fluorination reaction for 10-60 min. When the reaction is finished, remove the residual gas from the reactor.

[0009] 4) Repeat step 3) 1-5 times.

[0010] As a further preferred technical solution of the present invention, the molybdenum disulfide is a single-layer, multi-layer, or doped or modified molybdenum disulfide material.

[0011] As a further preferred technical solution of the present invention, in step 1), molybdenum disulfide is dried in a vacuum oven for 1-3 hours.

[0012] As a further preferred embodiment of the present invention, the fluorinated mixed gas is composed of a mixture of an inactive gas and fluorine gas.

[0013] As a further preferred embodiment of the present invention, the inactive gas is at least one of helium, neon, argon, krypton, xenon, radon, nitrogen, and carbon dioxide.

[0014] As a further preferred technical solution of the present invention, in step 3), before the fluorinated mixed gas is introduced into the reactor, the reactor is first purged with the inactive gas.

[0015] As a further preferred embodiment of the present invention, the number of inflation and replacement cycles is at least three.

[0016] As a further preferred technical solution of the present invention, in step 3), the temperature of the fluorination reaction is 0-40℃.

[0017] According to another aspect of the present invention, the present invention also provides a molybdenum difluoride fluorinated material, which is prepared by the method described in any of the above-mentioned methods.

[0018] Compared with existing traditional methods that improve the antioxidant capacity of MoS2 by preparing defect-free high-quality MoS2, the preparation method of the present invention is significantly simpler and more efficient, and reduces the production process cost, which is expected to realize the large-scale practical production and application of MoS2. At the same time, the fluorine-containing chemical bonds introduced by the present invention have higher stability, thus exhibiting higher antioxidant capacity compared with defect-free high-quality MoS2, while also synergistically enhancing the self-lubricating ability of MoS2. Attached Figure Description

[0019] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.

[0020] Figure 1 XPS curves of samples prepared for Comparative Example 1 (original MoS2) and Example 3 (fluorinated MoS2).

[0021] Figure 2 This is a comparison chart showing the increase in oxygen content before and after wet treatment for samples prepared in Comparative Example 1 (original MoS2) and Example 3 (fluorinated MoS2).

[0022] Figure 3 The graph shows a comparison of the increase in oxygen content before and after wet treatment for the fluorinated MoS2 samples prepared in Comparative Examples 2, 3 and Example 3.

[0023] Figure 4 The graph shows a comparison of the increase in oxygen content before and after wet treatment for the fluorinated MoS2 samples prepared in Comparative Example 4 and Examples 3 and 10.

[0024] Figure 5 XRD patterns of samples prepared for Comparative Example 1 (fluorinated MoS2) and Example 3 (fluorinated MoS2).

[0025] Figure 6 A comparison chart showing the self-lubricating ability of samples prepared for Comparative Example 1 (raw MoS2) and Example 3 (fluorinated MoS2) and crude oil (the base oil used in the self-lubricating test).

[0026] The objectives, features, and advantages of this invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0027] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0028] Unless otherwise defined, the technical terms used in the following embodiments have the same meanings as commonly understood by those skilled in the art to which this invention pertains. Unless otherwise specified, the experimental reagents used in the following embodiments are conventional biochemical reagents; and the experimental methods described are conventional methods.

[0029] Examples 1-13 below describe the preparation of fluorinated MoS2 samples with antioxidant and excellent self-lubricating properties according to the present invention.

[0030] Example 1:

[0031] The MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa, completing three nitrogen purgings. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 0.1%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the same fluorinated gas mixture was introduced again to continue the fluorination reaction for 1 hour. This process was repeated a total of 3 times.

[0032] Example 2:

[0033] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 1%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0034] Example 3:

[0035] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0036] Example 4:

[0037] The MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 10%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0038] Example 5:

[0039] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 20%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0040] Example 6:

[0041] MoS2 raw material was placed in a vacuum oven at 60°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0042] Example 7:

[0043] MoS2 raw material was placed in a vacuum oven at 90°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0044] Example 8:

[0045] MoS2 raw material was placed in a vacuum oven at 150°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0046] Example 9:

[0047] MoS2 raw material was placed in a vacuum oven at 180°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times.

[0048] Example 10:

[0049] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of one fluorination cycle.

[0050] Example 11:

[0051] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of two times.

[0052] Example 12:

[0053] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of four times.

[0054] Example 13:

[0055] MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25°C, and a reaction time of 1 hour. After one reaction cycle, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of 5 times.

[0056] As a control experiment for Examples 1-13 above, Comparative Examples 1-4 below are for the preparation of control samples.

[0057] Comparative Example 1:

[0058] The MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Nitrogen gas was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, with a reaction temperature of 25°C and a reaction time of 1 hour. After each reaction, the residual gas in the reactor was evacuated, and the same nitrogen gas was introduced again to continue the fluorination reaction for 1 hour. This process was repeated a total of three times. The final product was an unfluorinated MoS2 sample, which, compared to the original MoS2 before the reaction, was...

[0059] Comparative Example 2:

[0060] MoS2 raw material (undried) was directly placed into a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was then evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 25 °C, and a reaction time of 1 h. After one reaction, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another 1 h. This process was repeated a total of 3 times. Finally, a fluorinated MoS2 sample with a destroyed layered structure was obtained.

[0061] Comparative Example 3:

[0062] MoS2 raw material was placed in a vacuum oven at 120℃ for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa, a reaction temperature of 100℃, and a reaction time of 1 hour. After one reaction, the residual gas in the reactor was evacuated, and the fluorinated gas mixture was reintroduced to continue the fluorination reaction for another hour. This process was repeated a total of three times. The final product was a fluorinated MoS2 sample with a destroyed layered structure.

[0063] Comparative Example 4:

[0064] The MoS2 raw material was placed in a vacuum oven at 120°C for 2 hours to thoroughly dry and remove moisture and other impurities. The dried MoS2 was then placed in a fluorination reactor. Nitrogen gas was introduced into the reactor, and the gas was evacuated until the pressure inside the reactor reached 100 Pa. This nitrogen purging process was repeated three times. Fluorine and nitrogen gas were introduced into a gas mixing vessel at a rate of 0.2 L / min to prepare a fluorinated gas mixture with a fluorine gas fraction of 5%. This fluorinated gas mixture was then introduced into the reactor at a rate of 0.2 L / min, reaching a pressure of 20 kPa. The reaction temperature was 25°C, and the reaction time was 3 hours.

[0065] The prepared samples and control samples were subjected to the following experimental tests:

[0066] Experimental Example 1:

[0067] The samples provided in Examples 1-13 and Comparative Examples 1-4 were subjected to antioxidant and self-lubricating ability tests under the same conditions. The antioxidant ability test conditions were as follows: 100 mg of sample was placed in a constant temperature and humidity chamber (temperature 30°C, humidity 88%) for 24 h. XPS and other tests were used to characterize the increase in oxygen content in fluorinated MoS2 before and after wet treatment, thereby evaluating the antioxidant ability of fluorinated MoS2. The XPS test results for the samples prepared in Comparative Example 1 and Example 3 are provided in [reference needed]. Figure 1As shown. Self-lubricating ability test conditions: The sample was ultrasonically dispersed in the base oil at a concentration of 1.5 mg / ml. The friction test load was 30 N, displacement 5 mm, speed 10 mm / s, and time 1800 s. The corresponding friction coefficient was obtained to evaluate the self-lubricating ability of the sample. Table 1 shows the statistical results of the increase in oxygen content (i.e., antioxidant performance) and friction coefficient (self-lubricating performance) of various samples before and after wet treatment. As shown in Table 1, the antioxidant and self-lubricating properties of the fluorinated MoS2 provided in Examples 1-13 are significantly better than those of the unfluorinated or fluorinated MoS2 provided in Comparative Examples 1-3.

[0068] Table 1. Test results of antioxidant and self-lubricating properties of different samples and control samples

[0069]

[0070]

[0071] Experimental Example 2:

[0072] The antioxidant properties of the fluorinated MoS2 provided in Example 3 and the unfluorinated (equivalent to the original) MoS2 provided in Comparative Example 1 were characterized, and the results are as follows: Figure 2 As shown. By Figure 2 It is evident that the antioxidant properties of fluorinated MoS2 are significantly superior to those of unfluorinated MoS2. This is because the unstable dangling bonds in the MoS2 sheets are easily oxidized and degraded in a humid environment; while the controlled fluorination modification in Example 3 introduces fluorine that directionally replaces unstable dangling bonds such as oxygen groups in the original MoS2 sheets, further forming highly stable fluorinated chemical bonds, thus exhibiting even higher antioxidant properties.

[0073] The antioxidant properties of the fluorinated MoS2 provided in Example 3 and the fluorinated MoS2 with disrupted layer structure provided in Comparative Examples 2-3 were characterized, and the results are as follows: Figure 3 As shown. By Figure 3 It is evident that the antioxidant properties of fluorinated MoS2 are significantly superior to those of fluorinated MoS2 with disrupted sheet structure. This is because in Comparative Example 2, the original MoS2 sheet surface adsorbs a large number of water molecules. Without high-temperature drying, these water molecules and fluorine gas readily react violently on the MoS2 sheet surface, thus destroying the sheet structure. In Comparative Example 3, the fluorination reaction is carried out at a high temperature (100℃), which is violent and uncontrollable, further damaging the sheet structure. Therefore, the disrupted sheet structure of the fluorinated MoS2 in Comparative Examples 2-3 exposes more dangling bonds, making it more susceptible to oxidative degradation in humid environments, resulting in poorer antioxidant properties.

[0074] Experimental Example 3:

[0075] The antioxidant properties of the fluorinated MoS2 provided in Examples 3 and 10, and the fluorinated MoS2 provided in Comparative Example 4, were characterized, and the results are as follows: Figure 4 As shown. By Figure 4 It can be seen that the antioxidant properties of the fluorinated MoS2 provided in Example 10 and the fluorinated MoS2 provided in Comparative Example 4 are not significantly different. This is because after the fluorination reaction time exceeds 1 hour, the fluorine gas is basically consumed and will not continue to react. Therefore, the antioxidant properties of fluorinated MoS2 prepared with a fluorination reaction time of 3 hours and 1 hour are essentially the same. However, Example 3 involved three staged fluorination reactions, with fresh fluorine gas introduced each time, allowing for continuous reaction with MoS2. Ultimately, the unstable dangling bonds of MoS2 were completely replaced to form stable fluorinated chemical bonds, resulting in better antioxidant properties.

[0076] Experimental Example 4:

[0077] In addition to the aforementioned advantages in antioxidant capacity, the fluorinated MoS2 of this invention exhibits a larger interlayer spacing due to the introduction of fluorine, further enhancing its self-lubricating ability. Figure 5 As can be seen, XRD tests show that the fluorinated MoS2 provided in Example 3 has a larger interlayer spacing than the unfluorinated MoS2 in Comparative Example 1; Figure 6 As can be seen, the friction test shows that the fluorinated MoS2 provided in Example 3 has a lower coefficient of friction than the unfluorinated MoS2 in Comparative Example 1, thus demonstrating greater application prospects in the field of nanocomposites and lubrication in combination with its antioxidant capacity.

[0078] While specific embodiments of the present invention have been described above, those skilled in the art should understand that these are merely illustrative examples, and various changes or modifications can be made to these embodiments without departing from the principles and essence of the present invention. The scope of protection of the present invention is defined only by the appended claims.

Claims

1. A method for preparing a molybdenum disulfide fluoride material, characterized in that, Includes the following steps: 1) Dry molybdenum disulfide thoroughly at 60-150℃, and then place it in the reactor; 2) Prepare a fluorinated mixed gas with a fluorine gas fraction of 0.1-20%; 3) Introduce the fluorinated mixed gas prepared in step 2) into the reactor in step 1) at a rate of 0.2-5 L / min until the pressure is 2-80 kPa, and carry out the fluorination reaction for 10-60 min. When the reaction is finished, remove the residual gas from the reactor. 4) Repeat step 3) 1-5 times.

2. The method for preparing molybdenum disulfide fluoride material according to claim 1, characterized in that, The molybdenum disulfide is a single-layer, multi-layer, or doped or modified molybdenum disulfide material.

3. The method for preparing molybdenum disulfide fluoride material according to claim 1, characterized in that, In step 1), molybdenum disulfide is dried in a vacuum oven for 1-3 hours.

4. The method for preparing molybdenum disulfide fluoride material according to claim 1, characterized in that, The fluorinated gas mixture is composed of an inactive gas and fluorine gas.

5. The method for preparing molybdenum disulfide fluoride material according to claim 4, characterized in that, The inactive gas is at least one of helium, neon, argon, krypton, xenon, radon, nitrogen, and carbon dioxide.

6. The method for preparing molybdenum disulfide fluoride material according to claim 5, characterized in that, In step 3), before introducing the fluorinated mixed gas into the reactor, the reactor is first purged with the inactive gas.

7. The method for preparing molybdenum disulfide fluoride material according to claim 6, characterized in that, The inflation and purging process should be performed at least three times.

8. The method for preparing molybdenum disulfide fluoride material according to claim 1, characterized in that, In step 3), the fluorination reaction is carried out at a temperature of 0-40℃.

9. A molybdenum disulfide fluoride material, characterized in that, It is prepared by the method described in any one of claims 1-8.

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