Method for preparing high-temperature lubricating material from high-temperature slag and application of high-temperature lubricating material

Abstract

The invention discloses a method for preparing a high-temperature lubricating material from high-temperature slag and application of the high-temperature lubricating material, and relates to the technical field of industrial solid waste utilization. According to the method, ferronickel slag is adopted as a main raw material and is converted into a high-temperature lubricant with excellent performance through high-temperature melting and water quenching processes, and the high-temperature lubricant is applied to the thermal forming machining process of alloy profiles such as high-temperature alloy and titanium alloy. According to the method, the resource utilization rate of the ferronickel slag can be effectively increased, soil and water pollution caused by stacking and landfill can be reduced, so that green resourceful treatment of the slag is realized, related cost can be greatly reduced by replacing an outsourced high-temperature lubricant, and remarkable economic and environmental benefits are achieved.

Description

Technical Field

[0001] This invention relates to the field of industrial solid waste utilization technology, specifically to a method for preparing high-temperature lubricating materials from high-temperature slag and its application. Background Technology

[0002] Nickel-iron slag is a major solid waste generated during the smelting of nickel-iron alloys. With the rapid development of my country's stainless steel industry, the annual output of nickel-iron slag has exceeded 30 million tons, and the historical accumulated stockpile exceeds hundreds of millions of tons, making it the fourth largest metallurgical solid waste after blast furnace slag, steel slag, and red mud.

[0003] Nickel-iron ore slag has unique chemical composition characteristics: extremely high MgO content (25-35%), relatively high SiO2 content (40-50%), and extremely low CaO content (<10%). It also contains small amounts of Al2O3 (5-10%), Fe2O3 (5-15%), and trace amounts of Cr2O3, MnO, NiO, etc. Its basicity (CaO / SiO2 mass ratio) is typically less than 0.2, classifying it as a typical acidic slag. This ultra-low basicity and high magnesium characteristic is fundamentally different from conventional blast furnace slag (basicity > 1.0) and steel slag (basicity > 2.5), posing a serious obstacle to its traditional resource utilization.

[0004] Nickel-iron ore slag, after water quenching, exhibits a glassy or semi-glassy structure, appearing as a grayish-green granular solid with certain potential activity. However, due to its MgO content far exceeding national standard limits, this potential activity is difficult to effectively utilize in traditional building materials applications. Therefore, developing high-value utilization technologies for nickel-iron ore slag is of significant economic and environmental importance for achieving green and sustainable development of the stainless steel industry, reducing environmental pollution, and conserving land resources.

[0005] In high-end manufacturing fields such as aerospace, nuclear power, and petrochemicals, the hot working processes (such as hot forging, hot extrusion, and hot rolling) of materials like titanium alloys, high-temperature alloys, and tungsten alloys need to be carried out in high-temperature environments. Titanium alloy forging temperatures are typically between 700℃ and 1100℃, with α-β type titanium alloys generally forging between 900℃ and 950℃. Traditional organic and graphite lubricants oxidize, decompose, or fail within this temperature range, failing to meet the demands of high-temperature lubrication.

[0006] Currently, high-temperature lubricating materials mainly include the following types: (1) Glass lubricants: lubrication is achieved by utilizing the softening and flow characteristics of glass at high temperatures, which has good high-temperature stability and lubrication effect. Most existing glass lubricants adopt borosilicate systems, and the raw materials are mainly industrial pure chemical reagents, such as quartz sand, boric acid, soda ash, magnesium oxide, etc., which have high preparation costs; (2) Layered solid lubricants: such as boron nitride, molybdenum disulfide, etc., although they have excellent high-temperature resistance, the preparation process is complicated and the cost is high. Although these lubricating materials perform well in high-temperature environments, they generally face high preparation costs, which limits their wider application. The existing technology discloses a glass lubricant with polyisobutylene, glyceryl monostearate, boron nitride glass powder, etc. as the main raw materials; at the same time, it discloses a glass protective lubricant for high-temperature alloys, whose main raw materials include surface-grown silica, modified bentonite / silica composite powder, high-alumina borosilicate glass, low-temperature lead-free glass and boron nitride. Current high-temperature lubricating materials mainly use expensive raw materials such as special ceramic powders (e.g., boron nitride) and glass powder, resulting in high costs.

[0007] In conclusion, developing a high-temperature lubricating material that uses industrial solid waste as raw material, is inexpensive, and has excellent performance is of great significance for realizing the high-value utilization of solid waste and reducing the cost of high-temperature processing. Summary of the Invention

[0008] To address the shortcomings of the aforementioned background technology, this invention provides a method for preparing high-temperature lubricating materials from high-temperature slag and its application. This method uses slag powder as raw material, supplemented with a network formation of specific components and proportions, and obtains the desired high-temperature lubricating material through melt water quenching, ball milling, and sieving.

[0009] The first objective of this invention is to provide a high-temperature lubricating material based on high-temperature slag, wherein the raw materials of the high-temperature lubricating material comprise the following components by mass percentage: Slag 30-80%, silica 0-45%, alumina 2-10%, sodium oxide 5-25%, boron oxide 3-25%, total mass percentage of all components 100%; The slag is nickel-iron slag.

[0010] Preferably, the raw materials also include: ZnO 0.1~6%, BaO 0.1~8% and / or K2O 0.1~6%.

[0011] Preferably, the slag is obtained according to the following steps: Nickel-iron ore slag with a total iron content of less than 10% by mass is screened to obtain raw materials with a particle size ≤ 2mm; Raw materials with a particle size ≤ 2 mm are wet ball-milled with ethanol at a mass ratio of 1:1, with a ball-to-material ratio of 4~10:1, a ball-milling time of 12~18 h, and a rotation speed of 350~450 r / min. The resulting slurry is then magnetically separated to reduce the metallic iron content to below 2%. The slag slurry after magnetic separation is dehydrated and dried to obtain slag.

[0012] The second objective of this invention is to provide a method for preparing a high-temperature lubricating material based on high-temperature slag, comprising the following steps: Weigh the raw materials according to the mass percentage, mix them evenly, melt them at 1300-1400℃ for 40-240 minutes, and then quench the molten product in cold water at 10-25℃. Subsequently, filter and separate the water-quenched product, and dry it to obtain nickel-iron slag-based water-quenched glass. After wet ball milling, nickel-iron slag-based water-quenched glass is dried, filtered, and sieved to obtain a high-temperature lubricating material based on high-temperature slag.

[0013] Preferably, the wet ball milling process includes ball milling nickel-iron slag-based water-quenched glass with ethanol at a mass ratio of 1:1, wherein the ball-to-material ratio is 4~10:1, the ball milling time is 12~18 h, and the rotation speed is 350~450 r / min.

[0014] Preferably, a 400-mesh sieve is used for the filtration and sieving process.

[0015] Preferably, the drying is carried out at 80–120°C for 2–8 hours.

[0016] The third objective of this invention is to provide an application of a high-temperature lubricating material based on high-temperature slag in the field of high-temperature lubrication.

[0017] The fourth objective of this invention is to provide a lubricating coating, which is prepared by dispersing a high-temperature lubricating material based on high-temperature slag in a solvent, wherein the solvent is water, anhydrous ethanol or acetone.

[0018] Compared with the prior art, the beneficial effects of the present invention are: This invention provides a method for preparing high-temperature lubricating materials from high-temperature slag and its application. This invention effectively reduces the environmental impact of nickel-iron slag, improves the resource utilization rate of slag, and achieves high-value conversion and reuse of waste. This invention significantly reduces the production cost of high-temperature lubricating materials, especially glass lubricating materials commonly used in thermoforming processes, giving them a more competitive economic advantage. The high-temperature lubricating materials provided by this invention have a wide applicable temperature range and can be used stably in high-temperature environments of 700-1300℃, meeting various high-temperature processing requirements. Attached Figure Description

[0019] Figure 1 (a) is the XRD of slag glass before transformation, and (b) is the XRD of slag glass after transformation (before transformation it is a crystalline phase, and after transformation it is an amorphous phase). Figure 2 This is a comparison curve of the coefficient of friction of Glass1 lubricant at 750°C and dry friction in Example 1; Figure 3 This is a comparison curve of the coefficient of friction of Glass 2 lubricant at 750°C and dry friction in Example 2; Figure 4 This is a comparison curve of the coefficient of friction of Glass3 lubricant at 750°C and dry friction in Example 3; Figure 5 This is a comparison curve of the coefficient of friction of Glass4 lubricant at 1000°C and dry friction in Example 4; Figure 6 This is a comparison curve of the coefficient of friction of Glass 5 lubricant at 1000°C and dry friction in Example 5; Figure 7 This is a comparison curve of the coefficient of friction of Glass6 lubricant at 1000°C and dry friction in Example 6; Figure 8 This is a comparison curve of the coefficient of friction of Glass1 lubricant at 1250°C and dry friction in Example 7; Figure 9 This is a comparison curve of the coefficient of friction of Glass2 lubricant at 1250°C and dry friction in Example 8; Figure 10 This is a comparison curve of the coefficient of friction of Glass3 lubricant at 1250°C and dry friction in Example 9; Figure 11 The morphology of Glass1 lubricant in Example 10 at (a1) 500℃, (b1) 600℃, (c1) 700℃, (d1) 800℃, (e1) 900℃, and (f1) 950℃ is shown. Figure 12 The morphology of Glass2 lubricant in Example 11 at (a2) 600℃, (b2) 700℃, (c2) 800℃, (d2) 900℃, (e2) 1000℃, and (f2) 1050℃ is shown. Figure 13 The morphology of Glass3 lubricant in Example 12 at (a3) ​​600℃, (b3) 800℃, (c3) 900℃, (d3) 1000℃, (e3) 1100℃, and (f3) 1200℃ is shown. Detailed Implementation

[0020] To enable those skilled in the art to better understand and implement the technical solutions of the present invention, the present invention will be further described below in conjunction with specific embodiments and accompanying drawings. However, the embodiments described are not intended to limit the present invention.

[0021] The purpose of this invention is to provide a method for preparing high-temperature lubricating materials from high-temperature slag and its application. This invention uses nickel-iron slag as the main raw material, and through high-temperature melting and water quenching processes, it transforms it into a high-performance high-temperature lubricant, which is then applied in the hot forming process of high-temperature alloys and titanium alloy profiles. This technology not only effectively improves the resource utilization rate of nickel-iron slag and reduces soil and water pollution caused by stockpiling and landfilling, thus achieving green resource utilization of slag, but also significantly reduces related costs by replacing purchased high-temperature lubricants, resulting in significant economic and environmental benefits.

[0022] To achieve the above objectives, a first aspect of the present invention provides a high-temperature lubricating material based on high-temperature slag, wherein the raw materials of the high-temperature lubricating material comprise the following components by mass percentage: Slag 30-80%, silica 0-45%, alumina 2-10%, sodium oxide 5-25%, boron oxide 3-25%, total mass percentage of all components 100%; The slag is nickel-iron slag.

[0023] The design mechanism of each component in this invention is as follows: Slag (30-80%) serves as the main substrate, providing a glassy network framework with good high-temperature stability and oxidation resistance, while simultaneously realizing the resource utilization of industrial waste; Silica (0-45%) serves as the network forging agent, forming a three-dimensional glassy network structure and providing a slip-resistant layer with low shear strength; Alumina (2-10%) serves as the network intermediate, improving the cross-linking degree of the glass network and enhancing the mechanical strength and load-bearing capacity of the lubricating film; Sodium oxide (5-25%) serves as the network modifier, breaking bridging oxygen bonds to reduce the melting point and viscosity of the system, enabling the lubricating material to have good fluidity at operating temperatures; Boron oxide (3-25%) forms a layered lubricating phase, providing interlayer slip lubrication effects, while also participating in the construction of the glass network and synergistically reducing the melting point of the system; The synergistic effect of each component forms a viscous glassy phase, which spreads and solidifies at the friction interface to form a continuous lubricating protective film, achieving lubrication performance over a wide temperature range.

[0024] The raw materials for the high-temperature lubricating material also include: ZnO 0.1~6%, BaO 0.1~8%, and / or K2O 0.1~6%. Zinc oxide, as an amphoteric oxide, improves the chemical stability of the glass and the adhesion of the lubricating film; barium oxide can improve high-temperature creep resistance and enhance the structural stability of the lubricating film; potassium oxide can further reduce the melting temperature and improve the thermal compatibility between the lubricating film and the substrate; the synergistic effect of the components forms a viscous glass phase, which spreads and solidifies at the friction interface to form a continuous lubricating protective film, achieving lubrication performance over a wide temperature range. In this invention, the slag is obtained according to the following steps: Nickel-iron ore slag with a total iron content of less than 10% by mass is screened to obtain raw materials with a particle size ≤ 2mm; Raw materials with a particle size ≤ 2 mm are wet ball-milled with ethanol at a mass ratio of 1:1, with a ball-to-material ratio of 4~10:1, a ball-milling time of 12~18 h, and a rotation speed of 350~450 r / min. The resulting slurry is then magnetically separated to reduce the metallic iron content to below 2%. The slag slurry after magnetic separation is dehydrated and dried to obtain slag.

[0025] A second aspect of this invention provides a method for preparing a high-temperature lubricating material based on high-temperature slag, comprising the following steps: Weigh the raw materials according to the mass percentage, mix them evenly, melt them at 1300-1400℃ for 40-240 minutes, and then quench the molten product in cold water at 10-25℃. Subsequently, filter and separate the water-quenched product, and dry it to obtain nickel-iron slag-based water-quenched glass. After wet ball milling, nickel-iron slag-based water-quenched glass is dried, filtered, and sieved to obtain a high-temperature lubricating material based on high-temperature slag.

[0026] From the perspective of the preparation mechanism, the stable use of this lubricating material in high-temperature environments is mainly based on the following aspects: First, the pretreatment of the slag raw material ensures the purity and uniformity of the material. Screening and wet ball milling refine the slag to the micron level, significantly increasing the specific surface area and allowing for sufficient contact and reaction of the components during subsequent melting. Magnetic separation reduces the metallic iron content to below 2%, eliminating glass network defects caused by the presence of metal particles and improving the overall stability of the lubricating material.

[0027] Secondly, the high-temperature melting process of 1300–1400℃ is crucial for forming a stable glassy network structure. At this temperature, SiO2 and Al2O3 in the slag are fully melted and mixed with the added components, and silicon-oxygen tetrahedra and aluminum-oxygen ligands interconnect to form a three-dimensional network framework. Network modifiers such as Na2O and B2O3 are uniformly dispersed within it, breaking some bridging oxygen bonds and reducing the degree of network polymerization. A holding time of 40–240 minutes ensures the homogenization of the melt, eliminating component segregation and bubble defects, resulting in a dense and uniform glass network structure. This network structure formed at extremely high temperatures inherently possesses excellent high-temperature stability, laying the foundation for the material to maintain structural integrity at operating temperatures.

[0028] Secondly, water quenching is the core process for obtaining the amorphous glass phase. The molten product solidifies at an extremely rapid cooling rate (rapid cooling to 10–25°C), inhibiting crystal nucleation and growth, and maintaining the material's disordered glassy structure. This amorphous structure lacks weak points such as grain boundaries, avoiding failure modes such as grain boundary slip, grain growth, and phase transformation that easily occur in crystalline materials at high temperatures. Simultaneously, glassy materials possess an isotropic and continuous network structure, allowing them to flow and spread uniformly upon softening at high temperatures, forming a dense and continuous lubricating film layer, unlike crystalline materials which exhibit localized melting or structural abrupt changes.

[0029] Finally, wet ball milling grinds the water-quenched glass into a fine powder, improving the material's reactivity and spreadability during use. The fine glass particles soften rapidly under frictional heat and melt and flow at the friction interface, promptly filling micro-cracks and pits caused by wear, forming a self-healing lubricating protective layer. This viscous glass phase maintains a certain fluidity at high temperatures to achieve lubrication, while its stable network structure prevents complete flow failure, thus providing effective lubrication continuously over a wide temperature range.

[0030] The wet ball milling process includes ball milling nickel-iron slag-based water-quenched glass with ethanol at a mass ratio of 1:1, wherein the ball-to-material ratio is 4~10:1, the ball milling time is 12~18 h, and the rotation speed is 350~450 r / min.

[0031] During the filtration and sieving process, a 400-mesh sieve is used to obtain lubricating materials with a particle size of less than 40 μm.

[0032] The drying process involves drying at 80–120°C for 2–8 hours.

[0033] A third aspect of the present invention provides a lubricating coating, which is prepared by dispersing a high-temperature lubricating material based on high-temperature slag in a solvent, wherein the solvent is water, anhydrous ethanol or acetone.

[0034] For example, the pretreatment process for nickel-iron ore slag used in this invention includes steps such as screening, magnetic separation, wet ball milling, and subsequent drying. First, the slag is sequentially screened and magnetically separated, with the portion containing more than 20% total iron being separated and recycled; while the slag with a total iron content below 10% is further screened to obtain raw material with a particle size ≤ 2mm. Subsequently, wet ball milling is performed at a slag-to-ethanol mass ratio of 1:1, a ball-to-material ratio of 4-10:1, a milling time of 12-18 hours, and a rotation speed of 350-450 r / min. Afterward, the resulting slurry undergoes deep magnetic separation to reduce the metallic iron content to below 2%. Finally, the magnetically separated slag slurry is dehydrated and dried to obtain dried slag powder with the following composition by mass percentage: SiO2 47.59%, MgO 30.72%, Fe2O3 8.01%, Al2O3 6.63%, CaO 4.66%, Cr2O3 0.93%, and MnO 0.51%; thus achieving efficient recovery and resource utilization of valuable components in the slag.

[0035] Subsequently, the obtained dry slag powder is used as raw material, supplemented with a network formation of specific components and proportions, and then quenched in molten water, ball milled and sieved to obtain the required high-temperature lubricating material.

[0036] Specifically, the composition, in oxide equivalents, consists of the following components: 30-80% slag, 0-45% silica or its precursor, 2-10% alumina or its precursor, 5-25% sodium oxide or its precursor, 3-25% boron oxide or its precursor, and 0.1-8% BaO or 0.1-6% K2O, ZnO 0.1-6%, wherein the precursors can be converted into the corresponding oxides during sintering or melting.

[0037] Subsequently, the products obtained after sieving and mixing different formulations are placed in a high-temperature furnace at 1300–1400°C for melting for 40–240 minutes, and the molten glass is quickly immersed in cold water at 10–25°C for water quenching. After water quenching, the resulting glass particles are collected, washed, filtered, and separated, and then dried at 80–120°C for 2–8 hours, preferably at 100°C for 4 hours, to obtain the final nickel-iron slag-based water-quenched glass. Finally, the water-quenched glass is subjected to the same wet ball milling operation, and then dried, filtered, and sieved to obtain the final nickel-iron slag-based water-quenched glass high-temperature lubricant product.

[0038] The resulting lubricant can be used directly as a dry powder solid lubricant, or it can be dispersed in a solvent as the main lubricating phase to form a lubricating coating, which can then be applied by spraying, brushing, or impregnation. The solvent is water, anhydrous ethanol, acetone, or other organic solvents.

[0039] The fourth aspect of this invention provides an application of a high-temperature lubricating material based on high-temperature slag in the field of high-temperature lubrication.

[0040] It should be noted that, unless otherwise specified, the experimental methods used in this invention are all conventional methods; and the reagents and materials used, unless otherwise specified, are all commercially available.

[0041] The lubricant preparation process in the following embodiments includes: The raw materials of high-temperature lubricating materials with different formulations were screened and mixed, and the resulting products were melted in a high-temperature furnace at 1400℃ for 60 minutes. The molten glass was then quickly immersed in cold water at 25℃ for water quenching. After water quenching, the resulting glass particles were collected, washed, and dried. The cooled reaction products were washed and filtered for separation, and then dried at 100℃ for 4 hours to obtain the final nickel-iron slag-based water-quenched glass. Finally, the water-quenched glass was subjected to the same wet ball milling operation, dried, filtered, and sieved through a 400-mesh sieve to obtain the final nickel-iron slag-based water-quenched glass high-temperature lubricant product.

[0042] Example 1: The prepared Glass1 lubricant, composed of 30% slag, 25% silica, 18% sodium oxide, 18% boron oxide, and 9% aluminum oxide, was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the operating temperature was 700℃, the load was 10N, the linear velocity was 3 mm / s, the frequency was 0.5Hz, and the operating time was 20 min.

[0043] Experimental data show that using Glass1 lubricant significantly improves friction conditions. Compared with no lubrication (average coefficient of friction 0.4672), the average coefficient of friction is 0.1981, a reduction of 57.62%, and the coefficient of friction is relatively stable. The friction coefficient curve is shown in the attached figure. Figure 2 As shown.

[0044] Example 2: The prepared Glass2 lubricant, composed of 30% slag, 35% silica, 11% sodium oxide, 10.8% boron oxide, 7% aluminum oxide, 0.1% zinc oxide, 0.1% barium oxide, and 6% potassium oxide, was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating were then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the operating temperature was 700℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the operating time was 20 min.

[0045] Experimental data show that using Glass2 lubricant can effectively improve friction conditions. Compared with no lubrication (average coefficient of friction 0.4672), the average coefficient of friction is 0.2298, a reduction of 50.83%. However, the coefficient of friction fluctuates significantly. The friction coefficient curve is shown in the attached figure. Figure 3 As shown.

[0046] Example 3: The prepared Glass3 lubricant, composed of 30% slag, 45% silica, 10% sodium oxide, 10% boron oxide, and 5% aluminum oxide, was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The paired spheres were Si3N4 spheres, the operating temperature was 700℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the operating time was 20 min.

[0047] Experimental data show that using Glass3 lubricant can improve friction conditions. Compared with no lubrication (average coefficient of friction 0.4672), the average coefficient of friction is 0.3595, a reduction of 23.05%. However, the coefficient of friction is not stable; the coefficient of friction curve is shown in the attached figure. Figure 4 As shown.

[0048] Example 4: The prepared Glass4 lubricant, composed of 50% slag, 25% sodium oxide, and 25% boron oxide, was sprayed onto a special steel (P91 steel) substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the temperature was 1000℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the running time was 20 min.

[0049] Experimental data show that using Glass4 lubricant effectively improves friction conditions. Compared with no lubrication (average coefficient of friction 0.2636), the average coefficient of friction is 0.1908, a reduction of 27.62%, and the coefficient of friction remains relatively stable. The friction coefficient curve is shown in the attached figure. Figure 5 As shown.

[0050] Example 5: The prepared Glass5 lubricant, composed of 70% slag, 10% sodium oxide, 5.9% boron oxide, 6% zinc oxide, 8% barium oxide, and 0.1% potassium oxide, was sprayed onto a special steel (P91 steel) substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the operating temperature was 1000℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the operating time was 20 min.

[0051] Experimental data shows that using Glass5 lubricant failed to improve friction and even increased friction. Compared to no lubrication (average coefficient of friction 0.2636), the average coefficient of friction was 0.3453, representing a 30.99% increase. The friction coefficient curve is attached. Figure 6 As shown.

[0052] Example 6: The prepared Glass6 lubricant, composed of 80% slag, 10% silica, 5% sodium oxide, 3% boron oxide, and 2% aluminum oxide, was sprayed onto a nickel-based superalloy (15NiCuMoNb) substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the operating temperature was 1000℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the operating time was 15 min.

[0053] Experimental data show that using Glass6 lubricant effectively improves friction conditions. Compared with no lubrication (average coefficient of friction 0.4718), the average coefficient of friction is 0.4255, a reduction of 9.80%. The friction coefficient curve is attached. Figure 7 As shown.

[0054] Example 7: The Glass1 lubricant prepared in Example 1 was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the temperature was 1250℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the running time was 20 min.

[0055] Experimental data show that using Glass3 lubricant can effectively improve friction conditions. Compared with no lubrication (average coefficient of friction 0.2623), the average coefficient of friction is 0.1998, a reduction of 23.83%, and the coefficient of friction is relatively stable. The coefficient of friction curve is shown in the attached figure. Figure 8As shown.

[0056] Example 8: The Glass2 lubricant prepared in Example 2 was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The paired spheres were Si3N4 spheres, the temperature was 1250℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the running time was 20 min. Ti-6Al-4V Experimental data show that using Glass2 lubricant can effectively improve friction conditions. Compared with no lubrication (average coefficient of friction 0.2623), the average coefficient of friction is 0.1631, a reduction of 37.82%, and the coefficient of friction is relatively stable. The friction coefficient curve is shown in the attached figure. Figure 9 As shown.

[0057] Example 9: The Glass3 lubricant prepared in Example 3 was sprayed onto a Ti-6Al-4V substrate to form a lubricating coating with a thickness of approximately 100 μm. The lubrication, tribology, and wear performance of the lubricant / coating was then evaluated using a GF-I-1200 tribometer. The dual spheres were Si3N4 spheres, the temperature was 1250℃, the load was 10 N, the linear velocity was 3 mm / s, the frequency was 0.5 Hz, and the running time was 20 min.

[0058] Experimental data show that using Glass3 lubricant can improve friction conditions to a certain extent. Compared with no lubrication (average coefficient of friction 0.2623), the average coefficient of friction is 0.2144, a reduction of 18.26%, and the coefficient of friction remains stable. The coefficient of friction curve is shown in the attached figure. Figure 10 As shown.

[0059] Example 10: The glass powder prepared using Glass1 as described in Example 1 was pressed into cylindrical samples with a diameter of 5 mm × 3-5 mm. These samples were placed on an alloy substrate and heated from room temperature to 1400 °C at a rate of 10 °C / min in air. The morphology and wetting angle changes of the samples were recorded in real time. (See [reference needed]). Figure 11 As shown.

[0060] At around 700℃, a significant volume expansion was observed in the Glass1 powder sample, with an expansion rate of approximately 150-200% of the initial volume. This phenomenon is attributed to the rapid release of residual gases (such as water vapor and microbubbles) inside the glass as the glass approaches its glass transition temperature (Tg), leading to foaming and expansion of the sample.

[0061] As the temperature continued to rise to 850-900℃, the expansion phenomenon gradually weakened, and the glass began to exhibit good fluidity. At 900℃, the wetting angle of the Glass1 sample decreased to approximately 35-45°, indicating that it has good wetting and spreading ability at typical hot working temperatures of titanium alloys.

[0062] Glass1 exhibits excellent fluidity within a temperature range of 900-950℃, with the wetting angle further reduced to below 10°, enabling the formation of a uniform lubricating film on the substrate surface.

[0063] Example 11: The glass powder prepared by Glass2 as provided in Example 2 was pressed into cylindrical samples with a diameter of 5 mm × 3-5 mm, placed on an alloy substrate, and heated from room temperature to 1400 °C at a rate of 10 °C / min in air. The morphology and wetting angle changes of the samples were recorded in real time. See [link to relevant documentation]. Figure 12 As shown.

[0064] The Glass2 sample began to soften at around 800℃ and exhibited volume expansion in the 900-950℃ temperature range, although the expansion was less pronounced than that of Glass1. This is because Glass2 has a higher SiO2 content (35%), resulting in a denser glass network structure and a slightly higher glass transition temperature.

[0065] As the temperature continues to rise to 1000℃, the expansion phenomenon weakens, and the glass begins to exhibit good fluidity, with a decrease in the wetting angle. Within the temperature range of 1000-1100℃, Glass2 exhibits excellent fluidity, with the wetting angle further decreasing to below 10°, enabling the formation of a uniform lubricating film on the substrate surface.

[0066] Example 12: The glass powder prepared using Glass3 as described in Example 3 was pressed into cylindrical samples with a diameter of 5 mm × 3-5 mm. These samples were placed on an alloy substrate and heated from room temperature to 1400 °C at a rate of 10 °C / min in air. The morphology and wetting angle changes of the samples were recorded in real time. (See [reference needed]). Figure 13 As shown.

[0067] Due to its highest SiO2 content (45%), the Glass3 sample exhibited a relatively higher softening temperature. It began to soften at around 950℃ without expansion. Upon further heating to 1100℃, the glass began to show significant fluidity, with the wetting angle decreasing to approximately 35-45°. Within the temperature range of 1100-1200℃, Glass3 exhibited stable fluidity, maintaining a wetting angle of 30-40°, and was able to form a uniform lubricating film on the substrate surface.

[0068] To illustrate the performance of the lubricating material provided by this invention, it will be described in conjunction with the accompanying drawings.

[0069] Figure 1 In the middle, (a) is the XRD of pure slag glass before transformation, and (b) is the XRD of slag glass after transformation (the phase before transformation is crystalline, and the phase after transformation is amorphous). Figure 1 As shown in (a), the sample exhibits multiple sharp diffraction peaks, indicating that it has a crystal structure containing multiple crystal phases such as magnesium olivine, iron oxide, calcium oxide and olivine. Figure 1 As shown in (b), all three glass samples exhibit broad, diffuse peaks without any obvious sharp diffraction peaks, proving that the material has been transformed into an amorphous glass phase.

[0070] Although embodiments of the present invention have been shown and described above, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A high-temperature lubricating material based on high-temperature slag, characterized in that, The raw materials for the high-temperature lubricating material include the following components by mass percentage: Slag 30-80%, silica 0-45%, alumina 2-10%, sodium oxide 5-25%, boron oxide 3-25%, total mass percentage of all components 100%; The slag is nickel-iron slag.

2. The high-temperature lubricating material based on high-temperature slag according to claim 1, characterized in that, The raw materials also include: ZnO 0.1~6%, BaO 0.1~8% and / or K2O 0.1~6%.

3. The high-temperature lubricating material based on high-temperature slag according to claim 1, characterized in that, The slag is obtained according to the following steps: Nickel-iron ore slag with a total iron content of less than 10% by mass is screened to obtain raw materials with a particle size ≤ 2mm; Raw materials with a particle size ≤ 2 mm are wet ball-milled with ethanol at a mass ratio of 1:1, with a ball-to-material ratio of 4~10:1, a ball-milling time of 12~18 h, and a rotation speed of 350~450 r / min. The resulting slurry is then magnetically separated to reduce the metallic iron content to below 2%. The slag slurry after magnetic separation is dehydrated and dried to obtain slag.

4. A method for preparing a high-temperature lubricating material based on high-temperature slag as described in any one of claims 1 to 3, characterized in that, Includes the following steps: Weigh the raw materials according to the mass percentage, mix them evenly, melt them at 1300-1400℃ for 40-240 minutes, and then quench the molten product in cold water at 10-25℃. Subsequently, filter and separate the water-quenched product, and dry it to obtain nickel-iron slag-based water-quenched glass. After wet ball milling, nickel-iron slag-based water-quenched glass is dried, filtered, and sieved to obtain a high-temperature lubricating material based on high-temperature slag.

5. The method for preparing high-temperature lubricating material based on high-temperature slag according to claim 4, characterized in that, The wet ball milling process includes ball milling nickel-iron slag-based water-quenched glass with ethanol at a mass ratio of 1:1, wherein the ball-to-material ratio is 4~10:1, the ball milling time is 12~18 h, and the rotation speed is 350~450 r / min.

6. The method for preparing high-temperature lubricating material based on high-temperature slag according to claim 4, characterized in that, A 400-mesh sieve is used for the filtration and screening process.

7. The method for preparing high-temperature lubricating material based on high-temperature slag according to claim 4, characterized in that, The drying process involves drying at 80–120°C for 2–8 hours.

8. The application of the high-temperature lubricating material based on high-temperature slag as described in any one of claims 1 to 3 in the field of high-temperature lubrication.

9. A lubricating coating, characterized in that, The lubricating coating is prepared by dispersing the high-temperature lubricating material based on high-temperature slag as described in any one of claims 1 to 3 in a solvent, wherein the solvent is water, anhydrous ethanol or acetone.

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