Abrasive pre-treatment method and spectrum filter

Abstract

The embodiment of the present application provides an abrasive pretreatment method and a spectrometer. The abrasive pretreatment method is implemented by the spectrometer. The abrasive pretreatment method includes the following steps: pouring used oil into the filter space; adding a solvent to the filter space to dissolve and dilute the used oil, and then filtering; using a solvent to ultrasonically clean the abrasive on the filter membrane; using a solvent to rinse the abrasive; heating and drying the abrasive. The above-mentioned abrasive pretreatment method, by dissolving and diluting the used oil in the filter space, not only reduces the used oil attached to the abrasive, but also dilutes the high-viscosity used oil, making the filtration smoother, avoiding excessive filtration time or filter membrane clogging, so that the abrasive in the used oil is smoothly deposited on the filter membrane; ultrasonically cleaning the abrasive deposited on the filter paper ensures that the used oil in the surface contour of the abrasive is completely dissolved; drying and heating can volatilize the solvent on the surface of the abrasive.

Description

Technical Field

[0001] The present application relates to the technical field of oil monitoring, and in particular to an abrasive pre-treatment method and a spectrometer. Background Art

[0002] Oil monitoring technology is a technology that "draws blood for physical examination" of mechanical equipment. By testing the physical, chemical, contamination and wear indicators of the lubricating oil in use, the oil quality information and wear information of the mechanical equipment can be obtained, thereby reflecting the overall operating status of the equipment. In order to determine the degree of wear, wear mechanism and wear location of mechanical equipment, in addition to the conventional abrasive analysis of the lubricating oil in use, sometimes it is necessary to perform electron microscope energy spectrum analysis on the wear metal particles in the oil to obtain the high-magnification surface morphology and element content of specific abrasive particles.

[0003] At present, the standard methods and literature related to electron microscope energy spectrum are all for conventional block samples or dry powder samples, and there is no pre-treatment method for electron microscope energy spectrum detection of wear metal particles in used lubricating oil. In order to perform electron microscope energy spectrum analysis on wear particles in oil, the technical solution usually adopted now is to prepare spectrum slices according to the detection items of iron spectrum analysis in oil monitoring technology, which mainly includes two categories: analytical iron spectrum method and filter spectrum method. Analytical iron spectrum method uses solvent to dissolve the used lubricating oil, and then separates and deposits the wear particles (mainly ferromagnetic wear particles) in the oil sample through a magnetic field; filter spectrum method also uses solvent to dissolve the used lubricating oil, but separates and deposits the wear particles in the oil sample through membrane filtration. After completing the preparation of the wear particle spectrum slice, use a nail stand with conductive glue on the surface to stick the wear particles from the spectrum slice (glass spectrum slice or filter membrane spectrum slice), and then put the nail stand with the wear particles on the electron microscope stage, and finally perform electron microscope energy spectrum detection and analysis.

[0004] The existing technical solutions can complete sample preparation and perform electron microscope energy spectrum detection on abrasive particles, but there are the following problems:

[0005] First, the microscopic morphology of the abrasive surface photographed by the electron microscope is not clear enough. The surface of the abrasive separated by the iron spectrum analysis generally contains residues of lubricating oil and chemical reagents added during the preparation of the spectrum (such as tetrachloroethylene, solvent gasoline, etc.). The residues of these two will cover the surface of the abrasive after drying. On the one hand, it will cover the local microscopic area of ​​the abrasive and affect the observation effect of the overall microscopic morphology of the abrasive; on the other hand, because the residues are not conductive after drying, it is not conducive to the abrasive receiving electrons emitted from the electron gun of the scanning electron microscope, which affects the overall imaging effect of the abrasive.

[0006] Second, the particle element content detected by the energy spectrum is not accurate enough. Because the energy spectrometer tests the element composition of the micro-area on the surface of the sample, the lubricating oil and chemical reagent residues cover the surface of the abrasive particles, which will cause the result of the energy spectrum detection to be not the actual result of the abrasive metal particles. It usually leads to a high content of non-metallic elements (C and O) in the abrasive particles, while the content of metal elements (such as Fe, Cu, Pb, Sn, Cr, Mn, etc.) in the abrasive particles that reflect the wear of the equipment friction pair is relatively low. Summary of the invention

[0007] The purpose of the embodiments of the present application is to provide an abrasive pre-treatment method and a spectrometer.

[0008] The present application provides a method for pre-treating abrasive particles, comprising the following steps:

[0009] Pour the used oil into the filter space;

[0010] Add solvent into the filtration space to dissolve and dilute the oil in use, and then filter it;

[0011] Using the solvent to ultrasonically clean the abrasive particles on the filter membrane;

[0012] washing the abrasive grains using the solvent;

[0013] The abrasive grains are heated and dried.

[0014] The above-mentioned abrasive pre-treatment method, by dissolving and diluting the used oil, not only reduces the used oil attached to the abrasive, but also dilutes the used oil with high viscosity, making the filtration smoother, avoiding too long filtration time or filter membrane clogging, and allowing the abrasive in the used oil to be smoothly deposited on the filter membrane; the abrasive deposited on the filter paper is ultrasonically cleaned to ensure that the used oil in the surface contour of the abrasive is completely dissolved; then a solvent is used for secondary washing again, thus ensuring that the used oil residue on the surface of the abrasive is thoroughly washed away; dry heating can evaporate the solvent on the surface of the abrasive.

[0015] In one embodiment, the method for filtering the used oil is a filtration spectrum method, using a funnel and a filter membrane to filter the used oil.

[0016] In one embodiment, the step of adding a solvent into the filtration space to dissolve and dilute the oil in use comprises:

[0017] The boiling point of the solvent is less than or equal to the first preset temperature.

[0018] In one embodiment, the solvent includes one of gasoline, kerosene, petroleum ether (30-60), petroleum ether (60-90), petroleum ether (90-120), toluene, xylene, tetrachloroethylene and acetone.

[0019] In one embodiment, the solvent includes one of petroleum ether (30-60) and acetone.

[0020] In one embodiment, the step of using the solvent to ultrasonically clean the abrasive particles on the filter membrane comprises:

[0021] After the oil is filtered, the filter holes at the bottom of the filter space are closed, the solvent is added into the filter space, and then the ultrasonic cleaning element is placed into the filter space.

[0022] In one embodiment, the step of washing the abrasive particles with the solvent comprises:

[0023] After the ultrasonic cleaning is completed, the filter hole at the bottom of the filter space is opened, and the solvent is added again to wash the abrasive particles on the filter membrane.

[0024] In one embodiment, the step of heating and drying the abrasive particles comprises:

[0025] The abrasive grains are dried by vacuum heating.

[0026] In one embodiment, the heating and drying temperature is greater than or equal to the first preset temperature, and the heating and drying temperature is less than or equal to the second preset temperature.

[0027] A spectrum filter, applied to the abrasive pretreatment method described in any one of the above embodiments, the spectrum filter comprising:

[0028] A filter part having a filter space for containing a mixture of the used oil and the solvent;

[0029] A filter membrane, located at the bottom of the filter space, for filtering the used oil in the filter space and blocking the abrasive particles in the used oil;

[0030] The ultrasonic cleaning element is movably placed in the mixture of used oil and solvent in the filtering space.

[0031] The above-mentioned spectrometer, by dissolving and diluting the used oil in the filtering space, not only reduces the used oil attached to the abrasive particles, but also dilutes the used oil with high viscosity, making the filtration smoother and avoiding the filtration time being too long or the filter membrane being blocked, so that the abrasive particles in the used oil are smoothly deposited on the filter membrane; the abrasive particles deposited on the filter paper are ultrasonically cleaned to ensure that the used oil in the surface contour of the abrasive particles is completely dissolved; the solvent on the surface of the abrasive particles can be volatilized by drying and heating.

[0032] Other features and advantages of the present disclosure will be set forth in the following description, or some features and advantages may be inferred or unambiguously determined from the description, or may be learned by implementing the above-mentioned technology of the present disclosure.

[0033] In order to make the above-mentioned objects, features and advantages of the present application more obvious and easy to understand, preferred embodiments are specifically cited below and described in detail with reference to the attached drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0035] Figure 1 A schematic diagram of the structure of the spectrum filter provided in the embodiment of the present application;

[0036] Figure 2 A schematic flow chart of the abrasive pre-treatment method provided in an embodiment of the present application. DETAILED DESCRIPTION

[0037] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. The components of the embodiments of the present application described and shown in the drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the application claimed for protection, but merely represents the selected embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without making creative work belong to the scope of protection of the present application.

[0038] In the present application, the terms "upper", "lower", "left", "right", "front", "back", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings. These terms are mainly used to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to have a specific orientation, or to be constructed and operated in a specific orientation.

[0039] In addition, some of the above terms may be used to express other meanings in addition to indicating orientation or positional relationship. For example, the term "on" may also be used to express a certain dependency or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in this application can be understood according to specific circumstances.

[0040] In addition, the terms "installed", "set", "provided with", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection, or a point connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be an internal connection between two devices, elements, or components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0041] In addition, the terms "first", "second", etc. are mainly used to distinguish different devices, elements or components (the specific types and structures may be the same or different), and are not used to indicate or imply the relative importance and quantity of the indicated devices, elements or components. Unless otherwise specified, "plurality" means two or more.

[0042] In one embodiment, a method for pre-treating abrasive particles includes the following steps: pouring the used oil 2 into the filter space; adding a solvent to the filter space to dissolve and dilute the used oil 2, and then filtering; using the solvent to ultrasonically clean the abrasive particles on the filter membrane 6; using the solvent to rinse the abrasive particles; and heating and drying the abrasive particles.

[0043] like Figure 1 As shown, a method for pre-treating abrasive particles comprises the following steps:

[0044] 110. Pour the used oil 2 into the filtering space. A filtering part 3, such as a circular funnel, is placed therein, and the space inside the circular funnel is the filtering space.

[0045] 120. Add a solvent to the filtration space to dissolve and dilute the used oil 2, and then filter it. By adding a solvent to dissolve and dilute the used oil 2, not only is there less used oil 2 attached to the abrasive particles, but the high viscosity of the used oil 2 can also be diluted, making the filtration smoother, avoiding too long filtration time or clogging of the filter membrane 6, so that the abrasive particles in the used oil 2 are smoothly deposited on the filter membrane 6. In one embodiment, the method for filtering the used oil 2 is a spectral filter method, using a funnel and a filter membrane 6 to filter the used oil 2, wherein the filter membrane 6 is arranged at the bottom of the internal space of the funnel, used to seal the filter hole at the bottom of the funnel, and connected to the waste liquid collection device through the filter hole, for example, connected to the waste liquid bottle 5.

[0046] In one embodiment, the step of adding a solvent to the filter space to dissolve and dilute the oil 2 in use includes: the boiling point of the solvent is less than or equal to the first preset temperature. In this embodiment, the first preset temperature is the highest boiling point that the solvent can select, and the first preset temperature is 60°C. In this way, the solvent is a low-boiling-point solvent. After the spectrum slice is prepared, the solvent attached to the abrasive particles can be evaporated as much as possible to avoid affecting the subsequent electron microscope energy spectrum detection results; if a high-boiling-point solvent is directly used and the prepared abrasive particles are heated at high temperature, it is easy to cause oxidation of the abrasive particles, which will not only affect the color and microscopic morphology of the abrasive particle surface, but also affect the element detection results of the energy spectrum. Low-boiling-point solvents can avoid these problems.

[0047] In one embodiment, the solvent includes one of gasoline, kerosene, petroleum ether (30-60), petroleum ether (60-90), petroleum ether (90-120), toluene, xylene, tetrachloroethylene and acetone. These solvents with better solubility can be dissolved and diluted in the oil 2 to improve the filtering effect.

[0048] In one embodiment, the solvent includes one of petroleum ether (30-60) and acetone. For solvents with good solubility, kerosene, toluene, xylene and tetrachloroethylene have high boiling points (all greater than 100°C) and cannot meet the requirements of low boiling points of solvents, so they are excluded; although the lowest boiling point of gasoline is only 30°C, its highest boiling point reaches 220°C, so it cannot be completely volatilized at low temperatures, so it is excluded; petroleum ether (60-90) and petroleum ether (90-120) also have high boiling points, which are not easy to completely volatilize at low temperatures, and are also excluded. Therefore, the suitable low-boiling point solvent is petroleum ether (30-60) or acetone. It is worth mentioning that although acetone has low toxicity, it can anesthetize nerves, so it is carried out in a fume hood during operation to avoid inhalation into the human body. In addition, petroleum ether only contains C and H elements, and does not contain O elements. For samples with high accuracy requirements for O element test results, petroleum ether (30-60) is selected as a solvent.

[0049] 130. Use the solvent to ultrasonically clean the abrasive particles on the filter membrane 6. This can accelerate the cleaning of the used oil 2 on the abrasive particles. Specifically, in one embodiment, after the used oil 2 is filtered, the filter hole at the bottom of the filter space is closed, the solvent is added to the filter space, and then the ultrasonic cleaning component is placed in the filter space. In one embodiment, the ultrasonic cleaning component 1 is an ultrasonic rod. After the oil 2 is filtered, add an appropriate amount of the same low-boiling point solvent to the funnel, keep the valve 4 closed, insert the ultrasonic rod with a smooth surface into the funnel, and ultrasonically clean the abrasive particles deposited on the filter membrane 6 to ensure that the used oil 2 in the surface contour of the abrasive particles is completely dissolved; after ultrasonic cleaning for a period of time, open the valve 4 to release the solvent.

[0050] 140. Use the solvent to rinse the abrasive particles. Specifically, in one embodiment, after the ultrasonic cleaning is completed, the filter holes at the bottom of the filter space are opened, and the solvent is added again to rinse the abrasive particles on the filter membrane 6, i.e., a secondary rinse is performed, so as to ensure that the lubricating oil residue on the surface of the abrasive particles is thoroughly rinsed.

[0051] 150. Heat and dry the abrasive particles. In this way, the solvent can be evaporated by heat. Especially when the solvent is a low boiling point solvent, the solvent on the abrasive particles can be evaporated by heating to a certain temperature. In one embodiment, the abrasive particles are vacuum heated and dried, for example, the prepared filter membrane 6 spectrum is placed in a vacuum oven, so that the environment of the abrasive particles is free of oxygen to prevent the surface of the abrasive particles from being oxidized. In one embodiment, the heating and drying temperature is greater than or equal to the first preset temperature, and the heating and drying temperature is less than or equal to the second preset temperature. In this way, the heating temperature is greater than or equal to the first preset temperature, that is, greater than or equal to the boiling point of the solvent, so that the solvent can be evaporated, and the heating temperature is less than or equal to the second preset temperature. The second preset temperature is the highest temperature to prevent the abrasive particles from being heated and oxidized. In this way, the heating temperature is low to prevent the surface of the abrasive particles from being oxidized. In one embodiment, the heating temperature is set to 60°C to 70°C. In one embodiment, the heating temperature is set to 65°C, which ensures that the solvent is evaporated and the surface of the abrasive particles is prevented from being oxidized.

[0052] The above-mentioned abrasive pre-treatment method, by dissolving and diluting the used oil 2, not only makes the used oil 2 attached to the abrasive less, but also can dilute the used oil 2 with high viscosity, so that the filtration is smoother, avoiding too long filtration time or clogging of the filter membrane 6, so that the abrasive in the used oil 2 is smoothly deposited on the filter membrane 6; the abrasive deposited on the filter paper is ultrasonically cleaned to ensure that the used oil 2 in the surface contour of the abrasive is completely dissolved; then a solvent is used for secondary washing again, so as to ensure that the used oil 2 residue on the surface of the abrasive is thoroughly washed away; dry heating can volatilize the solvent on the surface of the abrasive.

[0053] In order to verify the accuracy of the abrasive pretreatment method, steel and copper sheets were soaked in gear oil to simulate the wear metal particles in the oil. The steel and copper sheets were cut uniformly, and the surface dirt and oxide layer were removed with sandpaper, and surface indentations close to the typical abrasive size (10-50 μm) were left on the surface of the metal sheets. They were ultrasonically cleaned with distilled water, and then immediately vacuum dried and heated. The gear oil was the newly purchased gear oil Shell Omala S2 G 320. The test temperatures included: 25°C room temperature, 65°C vacuum drying and heating temperature, and the test solvents included: gasoline, petroleum ether (30-60), and acetone.

[0054] The samples were pre-treated and tested by electron microscope energy spectrum according to the existing technical scheme and the abrasive pre-treatment method of the present application. Sample No. 1 is a clean metal sheet without subsequent treatment; samples No. 2 to No. 4 are metal sheets soaked in gear oil and added with solvent for direct filtration, and dried at room temperature 25°C; samples No. 5 to No. 7 are metal sheets soaked in gear oil and added with solvent for direct filtration, and then the metal sheets are ultrasonically cleaned with solvent, and then the steel sheets are rinsed twice with solvent, and finally dried at 65°C using a vacuum dryer. The electron microscope energy spectrum test results of the steel sheet are shown in Table 1, and the electron microscope energy spectrum test results of the copper sheet are shown in Table 2.

[0055] Table 1: Electron microscope energy spectrum test results of steel sheets

[0056]

[0057] Table 2: Electron microscope energy spectrum test results of copper sheet

[0058]

[0059]

[0060] The results show that the use of the operating procedures and low-boiling point solvents of the abrasive pretreatment method of the present application has indeed achieved good results. The metal element content of the sample in the abrasive pretreatment method of the present application is significantly higher than that of the prior art, and is close to the element content of the metal sheet itself. Among them, petroleum ether (30-60) has the best effect and the highest content of metal elements. This is because petroleum ether is completely compatible with mineral gear oil (Shell Omala S2 G 320) and can be completely volatilized at 65°C; while the effect of acetone is relatively poor, because acetone can only partially dissolve mineral gear oil (Shell Omala S2G320), and its dissolution effect is better after ultrasonic vibration dispersion. The above-mentioned embodiment experiments prove the effectiveness of the abrasive pretreatment method of the present application.

[0061] like Figure 1 As shown, a filter spectrometer 100 is applied to the abrasive pretreatment method described in any of the above embodiments, and the filter spectrometer includes a filter part 3, a filter membrane 6 and an ultrasonic cleaning element 1. The filter part 3 has a filter space for accommodating a mixture of the used oil 2 and the solvent; the filter membrane 6 is located at the bottom of the filter space, and is used to filter the used oil 2 in the filter space and block the abrasive particles in the used oil 2; the ultrasonic cleaning element 1 is movably placed in the mixture of the used oil 2 and the solvent in the filter space.

[0062] The above-mentioned spectrometer 100, by dissolving and diluting the used oil 2 in the filtering space, not only reduces the used oil 2 attached to the abrasive particles, but also dilutes the used oil 2 with high viscosity, making the filtration smoother and avoiding the filtration time being too long or the filter membrane 6 being blocked, so that the abrasive particles in the used oil 2 are smoothly deposited on the filter membrane 6; the abrasive particles deposited on the filter paper are ultrasonically cleaned to ensure that the used oil 2 in the surface contour of the abrasive particles is completely dissolved; the solvent on the surface of the abrasive particles can be volatilized by drying and heating.

[0063] In one embodiment, the spectrometer 100 further includes a waste liquid bottle 5, a valve 4 and a suction filtration mechanism, wherein the waste liquid bottle 5 is connected to the filtration space, the valve 4 is used to block the communication channel between the waste liquid bottle 5 and the filtration space, and the waste liquid bottle 5 is also connected to the suction filtration mechanism, that is, the valve 4 controls the opening and closing of the filtration, and the suction filtration mechanism provides a suction function to improve the efficiency of the filtration, and the waste liquid bottle 5 is used to collect the filtered in-use oil 2. In one embodiment, the suction filtration mechanism includes a hose 7 and a suction filtration pump 8, one end of the hose 7 is connected to the suction filtration pump 8, and the other end is connected to the internal space of the waste liquid bottle 5.

[0064] In all the embodiments of the present application, "big" and "small" are relative, "more" and "less" are relative, and "up" and "down" are relative. The expressions of such relative terms are not elaborated in the embodiments of the present application.

[0065] It should be understood that the "in this embodiment", "in the embodiment of the present application" or "as an optional implementation" mentioned throughout the specification means that the specific features, structures or characteristics related to the embodiment are included in at least one embodiment of the present application. Therefore, "in this embodiment", "in the embodiment of the present application" or "as an optional implementation" appearing throughout the specification does not necessarily refer to the same embodiment. In addition, these specific features, structures or characteristics can be combined in one or more embodiments in any suitable manner. Those skilled in the art should also be aware that the embodiments described in the specification are all optional embodiments, and the actions and modules involved are not necessarily required for the present application.

[0066] In the various embodiments of the present application, it should be understood that the size of the serial numbers of the above-mentioned processes does not necessarily mean the order of execution. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.

[0067] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any person skilled in the art who is familiar with the present technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. A method for pre-treating abrasive particles, characterized in that: The steps include: A spectrometer is used to perform abrasive pretreatment operations, wherein the spectrometer comprises: A filter part having a filter space for containing a mixture of the used oil and the solvent; A filter membrane, located at the bottom of the filter space, for filtering the used oil in the filter space and blocking the abrasive particles in the used oil; An ultrasonic cleaning member is movably placed in the mixture of the used oil and solvent in the filtering space; Based on the filter spectrum method, the used oil is filtered using a funnel and the filter membrane, the space inside the funnel is the filter space, the filter membrane is used to seal the filter holes at the bottom of the funnel, and the used oil is poured into the filter space; Adding a solvent into the filtering space to dissolve and dilute the oil in use, and then filtering, wherein the boiling point of the solvent is less than or equal to a first preset temperature, and the first preset temperature is 60° C.; the solvent includes one of petroleum ether (30-60) and acetone; The abrasive particles on the filter membrane are ultrasonically cleaned using the solvent, wherein after the oil is filtered, the filter holes at the bottom of the filter space are closed, the solvent is added into the filter space, and then the ultrasonic cleaning element is placed into the filter space; The abrasive particles are rinsed with the solvent, wherein after the ultrasonic cleaning is completed, the filter holes at the bottom of the filter space are opened, and the solvent is added again to rinse the abrasive particles on the filter membrane; The abrasive particles are vacuum heated and dried, the heating and drying temperature is greater than or equal to the first preset temperature, and the heating and drying temperature is less than or equal to the second preset temperature, and the second preset temperature is set between 60°C and 70°C.

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