Online in-situ detection and analysis system for abrasion failure mechanism of wide-temperature-range lubricating material

By designing an online in-situ detection and analysis system including vacuum components, friction and wear testing units, Raman detection units, high-temperature heating units and upper computers, the problem of detecting the wear failure mechanism of lubricating materials under high temperature and vacuum environments is solved, and the problem of detecting the wear failure mechanism of lubricating materials is realized. Real-time detection of phase components of the wear surface of lubricating materials and accurate evaluation of material properties.

CN119394834APending Publication Date: 2025-02-07LANZHOU INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202411817053.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-11
Publication Date
2025-02-07

AI Technical Summary

Technical Problem

The prior art is difficult to effectively detect the wear and failure mechanism of lubricating materials in special environments such as high temperatures and vacuums, resulting in the inability to accurately guide the design of the material system and improve performance.

Method used

An online in-situ detection and analysis system with a wide temperature domain lubricating material wear failure mechanism is designed, including vacuum components, friction wear testing unit, Raman detection unit, high-temperature heating unit and upper-level computer. Through Raman spectroscopy measurement and high-temperature vacuum environment simulation, Realize real-time detection of phase components of the wear surface of lubricating materials.

Benefits of technology

The system can monitor the changes in the phase components of the wear surface in real time within a wide temperature range, and combine the fluctuations of the friction coefficient and failure threshold to accurately reveal the wear resistance mechanism of material lubrication and damage failure mechanism, and guide the new wide temperature range solid lubrication resistance Development of grinding coating materials.

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Abstract

The invention discloses an online in-situ detection and analysis system for a wide-temperature-range lubricating material wear failure mechanism, which mainly comprises a vacuum high-temperature multi-environment friction and wear test part and an in-situ Raman detection part, and has an in-situ analysis equipment combination function and a vacuum, high-temperature and different-atmosphere environment controllable function. The system relates to three core function units of high vacuum, high temperature and in-situ Raman, and the difficulty lies in the compatibility of a high-temperature system and a high-vacuum system, the introduction of in-situ Raman and the compatibility of high vacuum and high temperature. According to the invention, three structural designs are adopted to overcome the difficulty: 1, the frictional wear experiment unit adopts a mechanical loading structural design; secondly, an open type design is adopted, a groove is formed in the upper part of a vacuum chamber, and a detection optical fiber of a Raman detection unit extends into the chamber; and thirdly, a circulating water cooling system is introduced, and a cooling water pipe is connected below the heating unit to cool the outer wall of the heating tank body.
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Description

Technical Field

[0001] The present invention belongs to the technical field of surface component state detection and analysis, and in particular relates to an online in-situ detection and analysis system for the wear failure mechanism of a lubricating material in a wide temperature range. Background Art

[0002] In the field of aerospace, some equipment works in special complex environments such as high temperature and vacuum. The working environment is relatively harsh and has high requirements for the performance of lubricating materials. It is necessary to study the wear failure mechanism of lubricating materials in the above environment. However, it is currently difficult to simulate the above environment on the ground, and friction tests are mainly carried out at room temperature / normal pressure. When testing at room temperature / normal pressure, the results obtained are quite different from the actual situation due to adsorption, oxidation, phase change and other reasons. As a result, the friction failure mechanism of solid lubricating materials used in vacuum, high temperature and other environments is currently unclear, and it is impossible to further guide the design of material systems and improve performance. Summary of the invention

[0003] In view of this, the purpose of the present invention is to overcome the current inability to detect and analyze the dynamic changes of the friction surface during the friction process in conventional friction and wear performance tests, and to reveal the friction and wear mechanisms of various organic, inorganic and other materials and pairs, especially for high temperature, vacuum and other environments. When the surface chemical state is measured when returning to room temperature / atmospheric environment, the results obtained are quite different from the actual situation, which brings difficulties to the exploration of the laws of friction and wear.

[0004] An online in-situ detection and analysis system for the wear failure mechanism of lubricating materials in a wide temperature range, comprising a vacuum component, a friction and wear test unit, a Raman detection unit, a high-temperature heating unit and a host computer; The vacuum assembly comprises a vacuum box, a mechanical pump and a molecular pump, and the vacuum box is evacuated by the mechanical pump and the molecular pump; The friction and wear test unit is fixed in a vacuum box, and includes a ball / pin fixture and a friction rod, the friction rod is connected to the ball / pin fixture, the friction rod is used to provide friction for the sample, and the ball / pin fixture is used to adjust the position of the friction rod; The Raman detection unit is fixed on the top of the vacuum box, the top of the vacuum box is connected to a vertical sleeve, the sleeve extends into the vacuum box, the bottom of the sleeve is high-transmittance glass, and the optical fiber lens of the Raman detection unit extends into the sleeve; the Raman detection unit is integrated with an XYZ three-way moving system, the XYZ three-way moving system controls the movement of the optical fiber lens in the sleeve, and performs in-situ observation and measurement of different positions of the wear mark; The high-temperature heating unit is arranged in a vacuum box, and the high-temperature heating unit is used to heat the sample; the high-temperature heating unit includes a heating tank and a cooling tank, the cooling tank is sleeved outside the heating tank, and a gap is left between the wall of the cooling tank and the wall of the heating tank, and the gap forms a cooling chamber; a resistance wire is arranged on the inner wall of the heating tank, and a reflection cover is formed on the inner wall of the heating tank, a motor is fixed at the center of the heating tank, the motor shaft is vertically upward, and a sample is connected to the top of the motor shaft, and the sample is close to the top position of the heating tank, and the motor is used to drive the sample to rotate; cooling water is introduced into the cooling chamber through a circulation system, and the cooling water circulates in the cooling chamber, and the cooling water cools the heating tank; a circular hole is opened in the center of the top of the heating tank and the cooling tank, and the friction rod is inserted into the heating tank through the circular hole and contacts the sample, and the circular holes of the heating tank and the cooling tank are sealed and connected to prevent the cooling water from overflowing; two temperature sensors are arranged in the heating tank, one is located inside the heating tank body for measuring the temperature of the inner cavity of the heating tank, and the other is located at the bottom of the sample for measuring the sample temperature; The host computer is electrically connected to the vacuum component, the friction and wear test unit, the Raman detection unit, and the high-temperature heating unit, and is used to control the start and stop and working parameters of each unit.

[0005] The ball / pin fixture includes a torque block, a scale, a left and right adjustment rocker, a support rod, a front and rear adjustment rocker, and a fixed pin; the ball / pin fixture adopts a series design and is supported by a support rod to ensure that the test ball / pin always fits the fixture without gaps and is not affected by thermal expansion and contraction due to temperature changes. The left end is a screw with a torque block, and the right side is a fixture hole and a fixed pin to adjust the length of the ball / pin so that it extends into the opening above the heating tank and contacts the sample; the rocker is adjusted to adjust the position of the friction frame according to the scale, and a fixed pin is configured to fix the friction test position, distance / radius. The sleeve and high-transparency glass are sealed with rubber rings and vacuum grease, and reinforced with stainless steel rings and screws.

[0006] It involves complex environments such as high temperature and vacuum, so a vacuum and high temperature multi-environment friction and wear test unit is needed that can simulate the high temperature of room temperature to 1000 ℃ and the vacuum complex environment of 10-4Pa.

[0007] In addition, the lubricating coating materials to be tested have the characteristics of many types of components, including organic resin binders and inorganic fillers such as graphite lubricants. It is necessary to select an online testing method with good detection capabilities for these materials. Among them, Raman spectroscopy measures Raman shifts, which can obtain information such as the structure, chemical bonds and composition of sample molecules, and realize quantitative and qualitative analysis of samples. It has a wide range of sensing capabilities for organic and inorganic materials, and has the advantages of non-destructive, no sample processing, high resolution, and no labeling. Therefore, it is preferred to equip the Raman in-situ detection component unit.

[0008] The present invention involves three core functional units: high vacuum, high temperature and in-situ Raman. The difficulty lies in the compatibility of the high temperature system and the high vacuum system, the introduction of in-situ Raman and the compatibility of high vacuum and high temperature. The present invention adopts three structural designs to overcome this difficulty. First, a mechanical loading structural design is adopted, which is more compatible with high vacuum and high temperature systems than electric loading; second, an open design is adopted to access the in-situ vacuum Raman detection component unit from the top of the chamber; third, a circulating water cooling system is introduced in the heating tank to reduce the outer wall temperature of the heating cavity and improve the compatibility of high temperature and high vacuum.

[0009] The ball / pin fixture of the present invention adopts a unique series elastic design to ensure that the test ball / pin is always matched with the fixture without gap, and is not affected by thermal expansion and contraction due to temperature changes. Equipped with a Raman in-situ detection component fiber optic probe, combined with an XYZ moving system, the specific position of the wear mark is measured in situ. A tank-type surround heating cavity is adopted, combined with a reflective cover on all sides to heat the sample evenly. At the same time, it is equipped with a circulating water cooling system to evenly cool the heating chamber and improve the service life of the instrument. The time required to heat to 1000°C is no more than 120 minutes. Two independent temperature sensors are installed: one is installed inside the cavity to directly test the temperature of the heating furnace, and the other is directly in contact with the bottom of the sample when testing at 1000°C to measure the temperature of the sample.

[0010] The beneficial effect of the present invention is to solve the difficult problem of evaluating the actual service performance of lubricating materials, monitor the real-time changes of the phase components of the wear surface during the friction process within a wide temperature range, and accurately reveal the lubrication and wear resistance mechanism and damage and failure mechanism of the material by combining the fluctuation of the friction coefficient and the failure threshold during the same period, so as to guide the development of new wide temperature range solid lubrication and wear-resistant coating materials and provide a basis for forming a systematic evaluation method. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 It is a schematic diagram of the structure of the test and analysis system of the present invention; Figure 2 It is a schematic diagram of the structure of the friction and wear testing unit of the present invention; Figure 3 It is a schematic diagram of the structure of the high temperature heating unit of the present invention; Figure 4 This is a diagram showing the friction test results of Example 1; Figure 5 This is the Raman spectrum detection diagram of Example 1; Figure 6 is the surface morphology of the wear scars of the two films in Example 2; Figure 7 This is a test result diagram of Example 2; In the figure: 1-friction and wear test unit; 2-Raman detection unit; 3-computer display; 4-high temperature heating unit; 5-molecular pump; 6-computer host; 7-mechanical pump; 8-chiller; 9-torque block; 10-scale; 11-left and right adjustment rocker; 12-support rod; 13-ball pin clamp; 14-front and rear adjustment rocker; 15-fixing pin; 16-heating tank; 17-cooling tank. DETAILED DESCRIPTION

[0012] The present invention discloses an online in-situ detection and analysis system for the wear failure mechanism of lubricating materials over a wide temperature range, and its main purpose is online testing and monitoring and analysis of friction and wear performance and surface state. The determination of the main technical index requirements also includes two parts. On the one hand, the equipment must be able to simulate the actual operating friction conditions in the task, including test temperature, vacuum, atmosphere, contact mode, speed, load, etc., while taking into account the accuracy of the test, and establishing the sensor test accuracy as the main technical indicator. On the other hand, the equipment can monitor and analyze the changes in the surface chemical state during the friction and wear process online through Raman spectroscopy, and can realize controllable detection of different materials, different positions, and different area sizes of wear marks.

[0013] An online in-situ detection and analysis system for the wear failure mechanism of lubricating materials in a wide temperature range comprises a vacuum component, a friction and wear test unit 1, a Raman detection unit 2, a high-temperature heating unit 4 and a host computer; the vacuum component comprises a vacuum box, a mechanical pump 7 and a molecular pump 5, and the vacuum box is evacuated by the mechanical pump 7 and the molecular pump 5.

[0014] The friction and wear testing unit 1 is fixed in a vacuum box. The friction and wear testing unit 1 includes a ball / pin fixture and a friction rod. The friction rod is connected to the ball / pin fixture. The friction rod is used to provide friction for the sample. The ball / pin fixture is used to adjust the position of the friction rod.

[0015] The Raman detection unit 2 is fixed on the top of the vacuum box, which is connected to a vertical sleeve that extends into the vacuum box. The bottom of the sleeve is high-transmittance glass, and the optical fiber lens of the Raman detection unit 2 extends into the sleeve. The Raman detection unit 2 is integrated with an XYZ three-way moving system that controls the movement of the optical fiber lens in the sleeve to perform in-situ observation and measurement of different positions of wear marks.

[0016] The high temperature heating unit 4 is arranged in the vacuum box, and the high temperature heating unit 4 is used to heat the sample; the high temperature heating unit 4 includes a heating tank 16 and a cooling tank 17, and the cooling tank 17 is sleeved outside the heating tank 16, and a gap is left between the tank wall of the cooling tank 17 and the tank wall of the heating tank 16, and the gap forms a cooling cavity; a resistance wire is arranged on the inner wall of the heating tank 16, and the inner wall of the heating tank 16 forms a reflective cover, and a motor is fixed at the center of the heating tank 16, and the motor shaft is vertically upward, and the top of the motor shaft is connected to the sample, and the sample is close to the top position of the heating tank 16, and the motor is used to drive the sample The sample rotates; cooling water is introduced into the cooling chamber through the circulation system, and the cooling water circulates in the cooling chamber to cool the heating tank 16; a circular hole is provided in the center of the top of the heating tank 16 and the cooling tank 17, and the friction rod is inserted into the heating tank 16 through the circular hole and contacts the sample, and the circular holes of the heating tank 16 and the cooling tank 17 are sealed to prevent the cooling water from overflowing; two temperature sensors are provided in the heating tank 16, one is located inside the heating tank 16 body for measuring the temperature of the inner cavity of the heating tank 16, and the other is located at the bottom of the sample for measuring the sample temperature.

[0017] The host computer is electrically connected to the vacuum component, the friction and wear test unit 1, the Raman detection unit 2, and the high-temperature heating unit 4. The host computer is used to control the start and stop and working parameters of each unit.

[0018] The ball / pin fixture includes a torque block 9, a scale 10, a left and right adjustment rocker 11, a support rod, a front and rear adjustment rocker 14, and a fixed pin 15; the ball / pin fixture adopts a series design and is supported by the support rod to ensure that the test ball / pin always fits with the fixture without gap and is not affected by thermal expansion and contraction due to temperature changes. The left end is a screw rod, which is equipped with a torque block 9, and the right side is a fixture hole and a fixed pin 15 to adjust the length of the ball / pin so that it extends into the opening above the heating tank 16 and contacts the sample; the rocker is adjusted to adjust the position of the friction frame according to the scale 10, and the fixed pin 15 is configured to fix the friction test position, distance / radius.

[0019] The sleeve and high-transmittance glass are sealed with rubber rings and vacuum grease, and reinforced with stainless steel rings and screws.

[0020] In the present invention, the friction machine component provides a material tribological performance detection function. Turn on the pump power supply, power on the friction machine, turn on the computer, and start the software; Vent to release the vacuum, open the chamber, clamp the sample, set the parameters, and start the experiment according to the prompts; close the cabin door, open the vacuum software, pump the mechanical pump, and when the vacuum degree reaches below 10 Pa, turn on the molecular pump until the vacuum degree reaches the test requirements and start the test; after the test is completed, turn off the molecular pump, stop the mechanical pump after the molecular pump turns to 0, and turn off the power to the friction machine. If sampling, click Vent to release the air. The chamber needs to maintain a certain vacuum degree if the testing machine is not used for a long time.

[0021] The high-temperature components provide a high-temperature test environment. You need to turn on the chiller first, set the target temperature, and start heating. After the test, turn off the heating, and then turn off the power and chiller power after the temperature drops.

[0022] The Raman spectroscopy component provides the phase detection function. Turn on the computer, turn on the spectroscopy host, and open the software for self-test for 3 minutes. Turn on the laser, 785 and 514 lasers, turn the key 90° clockwise, the 514 laser red light is on, and the 785 laser four indicators are yellow, which means it is turned on, about 5 minutes, 488 laser power is adjusted to the minimum, the laser power black switch O to I, and then turn the key 90° clockwise for about 15 minutes; if Raman is used alone, the microscope power supply needs to be turned on (the green button on the left side of the base); calibrate the sample silicon wafer, adjust the white light, turn the front knob to 1, turn the left knob to white light, adjust the software Swap to optical fiber or microscope (lecia), adjust the two options under Spectrometer state to the corresponding positions, and adjust Laser to the response option in the pop-up dialog box; focus, create a new test, set the test parameters, turn the front knob to 4 (laser position), adjust the left knob to laser azimuth, and click run to start the test; after the test is completed, turn off the laser, software, spectrometer host, computer, socket power, and microscope in turn.

[0023] In the above description, the equipment involves precision instruments and high temperature and high vacuum environments, and has some safety precautions: the order of power on and off cannot be wrong, and there are no special requirements for the order of microscopes; the laser has a preheating time. The four yellow lights of the 785 laser are on for full power, which is about 5 minutes. The red light of the 514 laser is on for full power, which is about 5 minutes. The red light of the 488 laser is on, which means that the power is on, and the yellow light is on when the output is completed. It takes 15 minutes after adjusting the power, and 15 minutes after each power adjustment. When shutting down 488, you need to adjust the power to the lowest first, and then shut down after the fan stops making noise; the equipment should not be turned on and off frequently. If someone uses it within 4 hours, it does not need to be shut down. If it is not used for half a year, it should be turned on once every 3 to 5 months; when doing high temperature tests, a layer of boron nitride powder needs to be brushed on the heating chamber, sample, and gasket. When clamping the sample, it needs to be loosened after tightening, and it needs to be lifted a little when clamping the fixture; this testing machine has strict requirements on the height and rotation radius of the friction specimen, the height is 12~13 mm, and the rotation radius is 17~19 mm; After power failure, the Raman probe may fall automatically. Please observe carefully to ensure that it does not collide with the friction parts.

[0024] According to the specific material characteristics and performance testing requirements, the following requirements are put forward for the main technical indicators of the equipment: 1. Friction upper limit: This indicator is the parameter of the friction test sensor, which refers to the upper limit of the sensor's friction test range. The friction range that this friction machine sensor can detect is 0 to 50 N; 2. Friction accuracy: Solid lubricating coating materials have extremely low friction coefficients. For example, the friction coefficient of MoS2-based coatings can reach 10 under vacuum. -3 The conventional loading is generally of the order of Newtons. To ensure that the friction coefficient can be accurately tested, the friction force accuracy is determined to be better than 1 mN. 3. Rotational motion mode and speed: Since many material friction performance test standards involved adopt the rotation mode, based on this, the equipment motion mode is determined to be the rotation mode, and the speed is 1 to 1000 rpm; 4. Temperature: The stable working temperature range is from room temperature to 1000 ℃, and the temperature control is ±5 ℃; 5. Vacuum degree: Generally speaking, the better the vacuum degree, the closer it is to the real ultra-vacuum environment in space. However, when the load has a high-temperature friction system, the vacuum degree should be better than 10 -4 Pa level is extremely difficult and the cost is greatly increased. -4 The vacuum degree of Pa can eliminate the influence of residual gases such as oxygen on the tribological properties of coating materials and the existing technical level, so the working pressure range is determined to be: 1×10 -4 Pa~atmosphere.

[0025] 6. Spectral resolution: There are many types of materials involved in the task. In order to ensure the accurate distinction of Raman signals of materials with similar peak positions, the minimum wavelength interval that the spectrometer can distinguish is determined, that is, the resolution is ≤1.5 cm -1 ; 7. Spot size: During the friction process, the width of the wear scar of the coating material is generally tens to hundreds of microns, while the local adhesion point or phase change point area is only a few microns. In order to fully detect the changes in the microstructure of the entire wear scar area, the detection spot diameter is set to be adjustable from 1 to 300 μm; 8. Spatial resolution of detection position: Detecting structural changes in local micro-areas requires precise positioning testing. In order to ensure the resolution of the micro-test area, the lateral resolution is determined to be <1 μm and the longitudinal resolution is <2 μm; 9. Excitation wavelength: There are many material systems involved in the task, including different types of organic and inorganic substances, different hybrid structures, etc. Different materials have different sensitivity to different excitation wavelengths. Using different excitation wavelengths for testing can more comprehensively and accurately reflect the information of the overall material. Therefore, three excitation wavelengths of 488 nm, 514 nm and 785 nm were determined.

[0026] like Figure 1 As shown in the figure, the system involves three core functional units: high vacuum, high temperature and in-situ Raman. The system consists of a high temperature friction and wear test unit, a high vacuum system (including a vacuum chamber and an exhaust system) and a Raman spectrometer.

[0027] The friction and wear test unit and the high temperature tank are placed in the vacuum chamber, and the Raman detection unit is placed on the vacuum chamber. When performing in-situ online detection, the sample is fixed on the sample table in the high temperature tank and a heating test is performed. At this time, the state changes of the sample surface in a vacuum or atmospheric environment as the ambient temperature increases can be detected. After setting the corresponding friction and wear test parameters and starting the friction and wear experiment, the changes in the sample surface state during the friction and wear process (high temperature / room temperature) in a vacuum or atmospheric environment can be detected, which makes it easier to reveal the friction and wear mechanism of the sample.

[0028] The above is only a preferred embodiment of the present invention. It should be pointed out that a person skilled in the art can make several improvements without departing from the principle of the present invention. These improvements should also be regarded as within the protection scope of the present invention.

[0029] The online in-situ detection and analysis system provided by the present invention is further described below in conjunction with embodiments.

[0030] Example 1 Turn on the power supply of the friction test component pump, power on the friction machine, turn on the computer, and start the software; Vent the vacuum and open the chamber, put the 9Cr18 sample plated with aC:H film into the sample holder, the dual ball is a 9Cr18 steel ball with a diameter of 8 mm, a height of 12 mm, a rotation radius of 18 mm, and the test parameters are set to 5 N, 1000 r / min, and a sampling frequency of 340 Hz; close the hatch and start the test according to the prompts; first run in for 2 minutes, and after the friction coefficient is stable, connect nitrogen to the chamber through the exhaust hole, and conduct a friction test in nitrogen for 10 minutes, then enter the air for 10 minutes, and then enter the nitrogen for 10 minutes. The results are as follows: Figure 4 During the test, the Raman spectrum of the wear surface was tested, and the results are shown in Figure 5 As shown in the figure, the wear scar morphology (a) and the corresponding Raman spectrum (b) of friction in air after the friction test in nitrogen, the wear scar morphology (c) and the corresponding Raman spectrum (d) of friction in nitrogen again, the midpoint (4, 5, 6) of the Raman spectrum corresponds to the test position (4, 5, 6) in the wear scar morphology. It can be seen from the Raman spectrum that the intensity of ID / IG increases further, indicating that the friction test process will destroy the complete structure of the graphene sheet. After a period of friction test (a short-term running-in in air and then a 10-min friction test in nitrogen), the ID / IG intensity in the air experiment further increased to 0.99-1.32, especially when it entered nitrogen again, its intensity value increased to 1.04-1.44.

[0031] Example 2 Turn on the power supply of the friction test component pump, power on the friction machine, turn on the computer, and start the software; Vent the vacuum and open the chamber, put the 9Cr18 sample plated with MoS2-Ti (MOST) and MoS2-Ti-TiB2 (MSTB) thin films into the sample holder, the dual ball is a GCr15 steel ball with a diameter of 8 mm, a height of 12 mm, a rotation radius of 18 mm, and the test parameters are set to 5 N, 1000 r / min, and a sampling frequency of 340 Hz; close the hatch, turn on the vacuum pump software, pump the mechanical pump, and turn on the molecular pump when the vacuum degree reaches below 10 Pa until the vacuum degree meets the test requirements, and start the test according to the prompts. According to the required test temperature, turn on the chiller, set the heating temperature, turn on the heating power supply, and start the experiment after the temperature stabilizes. During the experiment, the Raman spectrum of the wear scar surface was detected, and the surface morphology images of the wear scars of the two films are shown in the figure. Figure 6 As shown, a and b correspond to MOST and MSTB films respectively. The test results are shown in Figure 7 At room temperature (RT) or during heating at 100 °C, the -1 and ~410 cm -1 The characteristic peak of MoS2 appears near the layered unit layer, corresponding to the E 2g and interlayer A 1g The vibration indicates that the wear surface of the MOST film has a clear friction-induced ordering trend, but no oxidation occurs. The same is true for the MSTB film. However, when the MSTB film is tested at 300 °C, the Raman spectrum at 820 cm -1 The appearance of the vibration characteristic peak corresponding to MoO3 indicates that the film has been oxidized, which is related to the residual gas in the chamber and the oxygen element physically adsorbed on the surface of the film before the experiment.

[0032] The examples show that by performing in-situ Raman detection during the test process, the changes in the physical phase of the film surface during the test process can be observed in real time, and the lubrication principle and failure mechanism of the film can be better revealed. Moreover, it can avoid the situation where the results obtained are very different from the actual situation due to adsorption, oxidation, phase change, etc. when the surface chemical state is measured again in room temperature / atmospheric environment after the friction performance test is carried out in special composite environments such as high temperature and vacuum. This is more convenient to further guide the design of the material system and improve the service performance of the material.

Claims

1. An online in-situ detection and analysis system for the wear failure mechanism of lubricating materials over a wide temperature range, characterized in that: It includes vacuum components, friction and wear test unit, Raman detection unit, high temperature heating unit and host computer; The vacuum assembly comprises a vacuum box, a mechanical pump and a molecular pump, and the vacuum box is evacuated by the mechanical pump and the molecular pump; The friction and wear test unit is fixed in a vacuum box, and includes a ball / pin fixture and a friction rod, the friction rod is connected to the ball / pin fixture, the friction rod is used to provide friction for the sample, and the ball / pin fixture is used to adjust the position of the friction rod; The Raman detection unit is fixed on the top of the vacuum box, the top of the vacuum box is connected to a vertical sleeve, the sleeve extends into the vacuum box, the bottom of the sleeve is high-transmittance glass, and the optical fiber lens of the Raman detection unit extends into the sleeve; the Raman detection unit is integrated with an XYZ three-way moving system, the XYZ three-way moving system controls the movement of the optical fiber lens in the sleeve, and performs in-situ observation and measurement of different positions of the wear mark; The high-temperature heating unit is arranged in a vacuum box, and the high-temperature heating unit is used to heat the sample; the high-temperature heating unit includes a heating tank and a cooling tank, the cooling tank is sleeved outside the heating tank, and a gap is left between the wall of the cooling tank and the wall of the heating tank, and the gap forms a cooling chamber; a resistance wire is arranged on the inner wall of the heating tank, and a reflection cover is formed on the inner wall of the heating tank, a motor is fixed at the center of the heating tank, the motor shaft is vertically upward, and a sample is connected to the top of the motor shaft, and the sample is close to the top position of the heating tank, and the motor is used to drive the sample to rotate; cooling water is introduced into the cooling chamber through a circulation system, and the cooling water circulates in the cooling chamber, and the cooling water cools the heating tank; a circular hole is opened in the center of the top of the heating tank and the cooling tank, and the friction rod is inserted into the heating tank through the circular hole and contacts the sample, and the circular holes of the heating tank and the cooling tank are sealed and connected to prevent the cooling water from overflowing; two temperature sensors are arranged in the heating tank, one is located inside the heating tank body for measuring the temperature of the inner cavity of the heating tank, and the other is located at the bottom of the sample for measuring the sample temperature; The host computer is electrically connected to the vacuum component, the friction and wear test unit, the Raman detection unit, and the high-temperature heating unit, and is used to control the start and stop and working parameters of each unit.

2. The online in-situ detection and analysis system for the wear failure mechanism of lubricating materials over a wide temperature range according to claim 1 is characterized in that: The ball / pin fixture includes a torque block, a scale, a left and right adjustment rocker, a support rod, a front and rear adjustment rocker, and a fixing pin; The ball / pin fixture adopts a series design and is supported by a support rod to ensure that the test ball / pin always fits with the fixture without gap and is not affected by thermal expansion and contraction due to temperature changes. The left end is a screw with a torque block, and the right side is a fixture hole and a fixed pin to adjust the length of the ball / pin so that it extends into the opening above the heating tank and contacts the sample; adjust the rocker to adjust the position of the friction frame according to the scale, and configure a fixed pin to fix the friction test position, distance / radius.

3. The online in-situ detection and analysis system for the wear failure mechanism of lubricating materials over a wide temperature range according to claim 1 is characterized in that: The sleeve and the high-transmittance glass are sealed with rubber rings and vacuum grease, and reinforced with stainless steel rings and screws.

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