阅读说明：本技术 一种固体润滑薄膜的低温制备方法及应用 (Low-temperature preparation method and application of solid lubricating film ) 是由 赵剑波 崔岗 宗爱玲 滕文建 赵洪光 王真 韩彬 于 2020-08-19 设计创作，主要内容包括：本发明公开了一种固体润滑薄膜的低温制备方法,包括将工件安装在旋转式鼠笼箱中；旋转式鼠笼箱旋转可快速达到硫化物的形成温度；将氢气通入炉内,清理工件；将氩气通入炉内,升高工件温度；温度升至180℃时,将含硫气体通入炉内；停止供入各气体,待消耗完毕后,将电压降低至0V；继续冷却10-30min后,取出旋转式鼠笼箱及工件,将工件立即进行浸油处理,即在工件的表面制得硫化物固体自润滑薄膜。制备方法应用在离子电渗透工艺和\或离子镀工艺中。本发明提高工件升温速度,优化硫化物的沉积位置；降低固体润滑薄膜的成型温度,提高薄膜的生产效率,从而提高零件在高速、真空等严苛磨损工况下的服役寿命,降低生产成本,提高生产效益。(The invention discloses a low-temperature preparation method of a solid lubricating film, which comprises the steps of installing a workpiece in a rotary squirrel cage box; the rotary squirrel cage box can quickly reach the formation temperature of sulfides by rotation; introducing hydrogen into the furnace, and cleaning the workpiece; introducing argon into the furnace, and raising the temperature of the workpiece; when the temperature is raised to 180 ℃, introducing sulfur-containing gas into the furnace; stopping supplying each gas, and reducing the voltage to 0V after the gas is consumed; and (3) continuously cooling for 10-30min, taking out the rotary mouse cage and the workpiece, and immediately carrying out oil immersion treatment on the workpiece to obtain the sulfide solid self-lubricating film on the surface of the workpiece. The preparation method is applied to the ion electroosmosis process and/or the ion plating process. The invention improves the heating speed of the workpiece and optimizes the deposition position of the sulfide; the forming temperature of the solid lubricating film is reduced, and the production efficiency of the film is improved, so that the service life of parts under severe abrasion working conditions such as high speed, vacuum and the like is prolonged, the production cost is reduced, and the production benefit is improved.)

1. A low-temperature preparation method of a solid lubricating film is characterized by comprising the following steps: the method comprises the following steps:

s1, replacing a main shaft and an outer cover cage of the rotary mouse cage box (1), installing a workpiece (2) to be made into a film in the rotary mouse cage box, placing the rotary mouse cage box on a cathode disc (4) of a vacuum furnace (3), and connecting the outer cover of the vacuum furnace with a positive electrode; sealing the vacuum furnace and then vacuumizing to medium vacuum;

s2, the rotary type mouse cage box is pulled to rotate, the rotary type mouse cage box forms a hollow cathode effect, and the forming temperature of sulfides can be quickly reached;

s3, introducing hydrogen into the furnace, adjusting the voltage to 100-200V, and continuously cleaning the workpiece through discharging for 5-15 min;

s4, introducing argon into the furnace, adjusting the voltage to 300-600V, and raising the temperature of the workpiece by using cathode sputtering;

s5, when the temperature is raised to 180 ℃, introducing sulfur-containing gas into the furnace, and preserving the heat for 0.5-2.5 hours;

s6, stopping supplying each gas, and reducing the voltage to 0V after the gas is consumed;

and S7, after continuously cooling for 10-30min, taking out the rotary rat cage and the workpiece, and immediately carrying out oil immersion treatment on the workpiece to obtain the sulfide solid self-lubricating film on the surface of the workpiece.

2. The low-temperature production method of a solid lubricating film according to claim 1, characterized in that: the two ends of a main shaft (7) of the rotary mouse cage box penetrate out of the outer cover cage (8) and are fixed with the outer cover cage, the cross section of the outer cover cage is circular, the main shaft can rotate to drive the outer cover cage to rotate, the deposition position of sulfides can be optimized, and the solid films on the surface of a workpiece are distributed more uniformly.

3. The low-temperature production method of a solid lubricating film according to claim 2, characterized in that: both ends of the main shaft are fixedly connected with flywheels (9), the flywheels and shifting forks (10) are mutually fixed through transmission keys (11), and the shifting forks are rotatably arranged on upright columns (13) through shifting fork bearings (12); the upright posts are arranged on the bottom plate (14); and the shifting fork is shifted to drive the flywheel to store energy through the transmission key and drive the main shaft to rotate, and the main shaft drives the outer cover cage and the workpiece to rotate.

4. The low-temperature production method of a solid lubricating film according to claim 3, characterized in that: a vertical seat (15) for fixing the main shaft is arranged between the positioning sleeve and the flywheel, the main shaft is arranged on the vertical seat through a main shaft bearing (16), and the vertical seat is arranged on the bottom plate (14).

5. The low-temperature production method of a solid lubricating film according to claim 4, characterized in that: the bottom plate is provided with a T-shaped groove, the vertical seat and the upright post can move along the T-shaped groove, and the vertical seat and the upright post are positioned by a mounting bolt (17) and a mounting nut (18) after the distance is adjusted.

6. The low-temperature production method of a solid lubricating film according to claim 3, characterized in that: a shifting fork shaft (19) is fixedly connected to the shifting fork, and the shifting fork shaft and the inner ring of the shifting fork bearing are mutually fixed.

7. The low-temperature production method of a solid lubricating film according to claim 1, characterized in that: when a film is prepared in an inner hole of a workpiece, the workpiece is sleeved on the main shaft and is positioned by depending on the outer surface, the outer surface of the workpiece is abutted against the inner wall of the outer cover cage, a gap is formed between the inner hole of the workpiece and the main shaft, and the workpiece is clamped by a positioning sleeve (20); glow discharge occurs on the surface of the inner hole of the workpiece and the outer surface of the main shaft, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

8. The low-temperature production method of a solid lubricating film according to claim 1, characterized in that: when a film is prepared on the outer surface of a workpiece, the workpiece is sleeved on the main shaft and is positioned by depending on the inner hole, the inner hole of the workpiece is abutted against the main shaft, a gap is formed between the outer surface of the workpiece and the outer cover cage, and the workpiece is clamped by a positioning sleeve (20); glow discharge occurs between the outer surface of the workpiece and the inner wall of the outer cover cage, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

9. The low-temperature production method of a solid lubricating film according to claim 1, characterized in that: the pressure in the furnace is measured by a vacuum pressure gauge (5), and the temperature of the workpiece is measured by a thermocouple (6).

10. Use of a low temperature process for the preparation of a solid lubricating film according to claim 1, characterised in that: the preparation method is applied to the ion electroosmosis process and/or the ion plating process.

Technical Field

The invention relates to a preparation method and application of a solid lubricating film, in particular to a low-temperature preparation method and application of a solid lubricating film.

Background

The solid lubrication breaks through the limitation of liquid lubrication, the friction and the wear are reduced by the solid lubricants such as powder or films, and the working range of parts is expanded. Compared with grease lubrication, the solid lubricating material has stronger bearing capacity and wider application range. The solid lubricating material is commonly used in severe working conditions such as high speed, vacuum and the like, and can also form a composite self-lubricating material together with base materials such as metal, ceramic and the like, so that the service life of easily-worn parts such as spacecrafts, vehicles and the like is greatly prolonged, and the wide attention of scholars at home and abroad is attracted.

The solid lubricant forms a transfer film on the surface of the mating material during friction of the solid lubricant film, so that the friction is generated in the lubricant, thereby reducing the friction and reducing the abrasion. The solid lubricant is often used in the form of a thin film to reduce wear, and may also be used in the form of a block or powder. This is because the lubricating film prevents direct contact between the surfaces of the ground parts, and also reduces the shear strength of the contact thin layer, thereby greatly reducing the friction coefficient. Moreover, the self-lubricating film has good binding force with a substrate and has better adaptability.

Currently, solid lubricating materials commonly used are soft metals, laminates, polymers, and inorganic compounds. Sulfide films such as ferrous sulfide and molybdenum disulfide are common solid lubricating materials and have good tribological properties. By adopting a plasma-assisted deposition method, the sulfide film can be directly formed on the surface of the part in situ, and is more efficient than methods such as microwave, radio frequency, hydrothermal reaction, electrochemical deposition and the like. However, the preparation temperature of the sulfide self-lubricating film is higher than the tempering temperature of the part, and the treatment time is longer. For carbon steel and alloy steel which need high hardness, the low-temperature tempering temperature is 180 +/-10 ℃, and the treatment time is shortened as much as possible. The method comprises the steps of utilizing high-frequency pulse plasma diffusion equipment to perform surface nano-treatment on a sample by Badema and the like, and performing low-temperature ion sulfurization treatment, wherein the heat preservation temperature is 220 ℃, and the heat preservation time is 90 min. Maluge et al ionically sulfurize the 1Cr18Ni9Ti stainless steel bombarded by supersonic particles at 220 deg.C, keeping the temperature for 1.5h, cooling to room temperature, taking out the sample, and vacuum packaging. Chinese patent application No.: 201010298115.5, the temperature control range of the workpiece is 100-650 ℃, and the sulfurization time reaches 0.5-20 hours. Chinese patent application No.: 201610838384.3, the ion sulfurizing treatment temperature is 800-900 deg.C, and the time is 60-120 min. The application of sulfide solid lubrication technology has been greatly limited due to the higher processing temperature and processing time.

Disclosure of Invention

In order to solve the defects of the technology, the invention provides a low-temperature preparation method and application of a solid lubricating film.

In order to solve the technical problems, the invention adopts the technical scheme that: a low-temperature preparation method of a solid lubricating film comprises the following steps:

s1, replacing a main shaft and an outer cover cage of the rotary mouse cage box, installing a workpiece to be made into a membrane in the rotary mouse cage box, placing the rotary mouse cage box on a cathode disc of a vacuum furnace, and connecting an outer cover of the vacuum furnace with a positive electrode; sealing the vacuum furnace and then vacuumizing to medium vacuum;

s2, the rotary type mouse cage box is pulled to rotate, the rotary type mouse cage box forms a hollow cathode effect, and the forming temperature of sulfides can be quickly reached;

s3, introducing hydrogen into the furnace, adjusting the voltage to 100-200V, and continuously cleaning the workpiece through discharging for 5-15 min;

s4, introducing argon into the furnace, adjusting the voltage to 300-600V, and raising the temperature of the workpiece by using cathode sputtering;

s5, when the temperature is raised to 180 ℃, introducing sulfur-containing gas into the furnace, and preserving the heat for 0.5-2.5 hours;

s6, stopping supplying each gas, and reducing the voltage to 0V after the gas is consumed;

and S7, after continuously cooling for 10-30min, taking out the rotary rat cage and the workpiece, and immediately carrying out oil immersion treatment on the workpiece to obtain the sulfide solid self-lubricating film on the surface of the workpiece.

Furthermore, two ends of a main shaft of the rotary mouse cage box penetrate out of the outer cover cage and are mutually fixed with the outer cover cage, the section of the outer cover cage is circular, the main shaft can drive the outer cover cage to rotate by rotation, the deposition position of sulfides can be optimized, and the solid film on the surface of a workpiece is distributed more uniformly;

furthermore, two ends of the main shaft are fixedly connected with flywheels, the flywheels and the shifting forks are mutually fixed through transmission keys, and the shifting forks are rotatably arranged on the upright posts through shifting fork bearings; the upright post is arranged on the bottom plate; and the shifting fork is shifted to drive the flywheel to store energy through the transmission key and drive the main shaft to rotate, and the main shaft drives the outer cover cage and the workpiece to rotate.

Furthermore, a vertical seat for fixing the main shaft is arranged between the positioning sleeve and the flywheel, the main shaft is arranged on the vertical seat through a main shaft bearing, and the vertical seat is arranged on the bottom plate.

Furthermore, a T-shaped groove is formed in the bottom plate, the vertical seat and the upright post can move along the T-shaped groove, and the vertical seat and the upright post are positioned by the mounting bolt and the mounting nut after the distance is adjusted.

Furthermore, a shifting fork shaft is fixedly connected to the shifting fork, and the shifting fork shaft and the inner ring of the shifting fork bearing are fixed to each other.

Furthermore, when a film is prepared in an inner hole of the workpiece, the workpiece is sleeved on the main shaft and is positioned by the outer surface, the outer surface of the workpiece is abutted against the inner wall of the outer cover cage, a gap is formed between the inner hole of the workpiece and the main shaft, and the workpiece is clamped by the positioning sleeve; glow discharge occurs on the surface of the inner hole of the workpiece and the outer surface of the main shaft, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

Furthermore, when a film is prepared on the outer surface of the workpiece, the workpiece is sleeved on the main shaft and is positioned by the inner hole, the inner hole of the workpiece is abutted against the main shaft, a gap is formed between the outer surface of the workpiece and the outer cover cage, and the workpiece is clamped by the positioning sleeve; glow discharge occurs between the outer surface of the workpiece and the inner wall of the outer cover cage, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

The pressure in the furnace is measured by a vacuum pressure gauge, and the temperature of the workpiece is measured by a thermocouple.

A low-temperature preparation method of a solid lubricating film is applied to an ion electroosmosis process and/or an ion plating process.

The invention has the following beneficial effects: according to the invention, the workpiece is installed by adopting the rotary mouse cage box, so that a hollow cathode effect is formed, the heating speed of the workpiece is increased, and the deposition position of sulfide is optimized; reacting metal particles sputtered by a cathode with sulfur-containing gas to generate metal sulfide, and preparing a sulfide solid lubricating film on the surface of a workpiece; through the material design of the main shaft and the outer cover cage, the metal type of the sputtering cathode is designed, the metal sulfide type can be regulated and controlled, the sulfide with lower forming temperature is prepared, the forming temperature of the solid lubricating film is reduced, and the production efficiency of the film is improved, so that the service life of parts under the severe abrasion working conditions of high speed, vacuum and the like is prolonged, the production cost is reduced, the production benefit is improved, and the problems that in the prior art, the preparation temperature of the sulfide solid film is high, the processing time is long, and the production cost is overhigh and the like can be effectively solved.

Drawings

Fig. 1 is a schematic view of the overall structure of the present invention.

FIG. 2 is a schematic sectional view of the rotary rat cage for preparing a thin film in an inner hole of a workpiece.

FIG. 3 is a schematic cross-sectional view of the rotary rat cage for preparing a thin film on the outer surface of a workpiece.

FIG. 4 is a surface SEM topography of a solid lubricating film prepared according to the present invention.

FIG. 5 is a topographical view of a wear scar of a workpiece without a thin film.

FIG. 6 is a topographical view of abrasive swarf from a workpiece without a film.

FIG. 7 is a topographical view of a wear scar in a workpiece using a thin film.

FIG. 8 is a topographical view of a workpiece using a thin film abrasive grit.

In the figure: 1. a rotary mouse cage box; 2. a workpiece; 3. a vacuum furnace; 4. a cathode disk; 5. a vacuum pressure gauge; 6. a thermocouple; 7. a main shaft; 8. an outer cage; 9. a flywheel; 10. a shifting fork; 11. a drive key; 12. a fork bearing; 13. a column; 14. a base plate; 15. a vertical seat; 16. a main shaft bearing; 17. installing a bolt; 18. mounting a nut; 19. a fork shaft; 20. a positioning sleeve; 21. a vacuum pump.

Detailed Description

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

A low-temperature preparation method of a solid lubricating film comprises the following steps:

s1, as shown in fig. 1, the main shaft and the outer cover cage of the rotary type mouse cage case 1 are replaced, the workpiece 2 to be film-formed is mounted in the rotary type mouse cage case, the rotary type mouse cage case is placed on the cathode plate 4 of the vacuum furnace 3, and the vacuum furnace is covered with the positive electrode. The vacuum furnace is sealed and then pumped to medium vacuum by a vacuum pump 21; the pressure in the furnace is measured by a vacuum pressure gauge 5, and the temperature of the workpiece is measured by a thermocouple 6.

As shown in fig. 2, when a film is prepared in an inner hole of a workpiece, the workpiece is sleeved on a main shaft, the workpiece is positioned by depending on the outer surface, the outer surface of the workpiece is abutted against the inner wall of an outer cover cage, a gap is formed between the inner hole of the workpiece and the main shaft, and the workpiece is clamped by a positioning sleeve 20; glow discharge occurs on the surface of the inner hole of the workpiece and the outer surface of the main shaft, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

As shown in fig. 3, when a film is prepared on the outer surface of a workpiece, the workpiece is sleeved on the spindle, the workpiece is positioned by means of the inner hole, the inner hole of the workpiece is abutted against the spindle, a gap is formed between the outer surface of the workpiece and the outer cover cage, and the workpiece is clamped by the positioning sleeve 20; glow discharge occurs between the outer surface of the workpiece and the inner wall of the outer cover cage, cathode sputtering is generated, and a sulfide solid self-lubricating film is formed.

S2, the rotary type mouse cage box is pulled to rotate, the rotary type mouse cage box forms a hollow cathode effect, and the forming temperature of sulfides can be quickly reached;

s3, introducing hydrogen into the furnace, adjusting the voltage to 100-200V, and continuously cleaning the workpiece through discharging for 5-15 min;

s4, introducing argon into the furnace, adjusting the voltage to 300-600V, and raising the temperature of the workpiece by using cathode sputtering;

s5, when the temperature is raised to 180 ℃, introducing sulfur-containing gas into the furnace, and preserving the heat for 0.5-2.5 hours;

s6, stopping supplying each gas, and reducing the voltage to 0V after the gas is consumed;

and S7, after continuously cooling for 10-30min, taking out the rotary rat cage and the workpiece, and immediately carrying out oil immersion treatment on the workpiece to obtain the sulfide solid self-lubricating film on the surface of the workpiece.

By adjusting the materials of the main shaft and the outer cover cage and selecting the metal which is easy to sputter, such as TU2, sulfide with lower forming temperature is prepared, and a solid film can be formed at 180 ℃ or even lower temperature.

Both ends of a main shaft 7 of the rotary mouse cage box penetrate out of the outer cover cage 8 and are mutually fixed with the outer cover cage, the section of the outer cover cage is circular, the main shaft can drive the outer cover cage to rotate by rotation, the deposition position of sulfides can be optimized, and the solid film on the surface of a workpiece is distributed more uniformly;

both ends of the main shaft are fixedly connected with flywheels 9, the flywheels and shifting forks 10 are mutually fixed through transmission keys 11, and the shifting forks are rotatably arranged on upright columns 13 through shifting fork bearings 12; a shifting fork shaft 19 is fixedly connected to the shifting fork, and the shifting fork shaft and the inner ring of the shifting fork bearing are fixed with each other; the upright posts are arranged on the bottom plate 14; and the shifting fork is shifted to drive the flywheel to store energy through the transmission key and drive the main shaft to rotate, and the main shaft drives the outer cover cage and the workpiece to rotate. The friction between the shifting fork and the upright post can be reduced by the shifting fork bearing, so that the resistance cannot be increased for the rotation of the outer cover cage.

A vertical seat 15 for fixing and supporting the main shaft is arranged between the positioning sleeve and the flywheel, the main shaft is arranged on the vertical seat through a main shaft bearing 16, and the vertical seat is arranged on a bottom plate 14. The spindle bearing reduces friction and thus does not add resistance to the rotation of the outer cage.

A T-shaped groove is formed in the bottom plate, the vertical seat and the upright post can move along the T-shaped groove to adapt to the outer cover cages of different sizes, and the outer cover cages are positioned by the mounting bolts 17 and the mounting nuts 18 after the distance is adjusted.

The low-temperature preparation method of the solid lubricating film can be applied to an ion electroosmosis process and/or an ion plating process.

The surface topography of the solid film obtained in this example was examined as shown in FIG. 4, where the film had covered the surface of the workpiece and formed to have a build-up.

5-8 are comparison graphs before and after the workpiece adopts the solid lubricating film, and the solid lubricating film can be found to have excellent antifriction and antiwear performances. Wherein (a) the graph (fig. 5) and (B) the graph (fig. 6) show the appearance of the grinding marks and the grinding chips without the thin film, the deeper scratches exist at the A position, and the size of the grinding chips at the B position is larger. (c) The figures (fig. 7) and (D) and (fig. 8) show the appearance of the wear scar and the wear debris with the thin film, where the thin film is unchanged at C and the thin film forms aggregates at D at both ends of the wear scar.

The above embodiments are not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make variations, modifications, additions or substitutions within the technical scope of the present invention.